TWI640330B - Polyparaxylene organic polymer film coating process for intravascular catheter - Google Patents

Abstract

The invention relates to a polyparaxylene organic polymer thin film coating process for an intravascular catheter, which includes placing the intravascular catheter in a cabin of a batch type plasma vacuum coating equipment and applying vacuum, applying plasma technology, and Plasma technology was used, and the intravascular catheter was placed in the chamber of the parylene organic polymer vacuum coating equipment and evacuated to form a uniform parylene organic polymer film in the blood vessel by vapor deposition. Steps such as pores on the surface of the catheter. Thereby, the adhesion between the parylene organic polymer film and the intravascular catheter can be reliably improved, and the nano-grade parylene organic polymer film can be more tightly and uniformly coated on the intravascular catheter. Purpose within the pores of the surface.

Description

Polyparaxylene organic polymer film coating process for intravascular catheter

The invention relates to a polyparaxylene organic polymer film coating process for an intravascular catheter, and more particularly to a method for improving the adhesion between the polyparaxylylene organic polymer film and the intravascular catheter, and making nano-scale polymer The para-xylene organic polymer film can more closely and uniformly cover the parylene organic polymer film coating process in the pores on the surface of the intravascular catheter.

Nano-sized parylene organic polymer film has good bacteriostatic, dry lubrication and hydrophobic properties. It can be modified after coating on the surface of intravascular catheters (such as intravenous infusion needles). Intravascular catheters after coating The hydrophobic angle of the surface will be increased, allowing the blood to flow faster, reducing the risk of thrombosis caused by platelet adhesion of intravascular catheters, and increasing the anticoagulant efficacy of intravascular catheters. The characteristics of dry lubrication can reduce the damage to vascular tissues during intubation, prevent the occurrence of complications, reduce the pain of puncture, and slow the discomfort of the human body.

Traditionally, the intravascular catheter is used as the substrate, and it is thoroughly dried after being washed with pure water, and a nano-scale parylene organic polymer thin film layer is coated on the outermost layer; or the intravascular catheter is used as the substrate according to different needs. On the surface of the intravascular catheter, evenly coat a layer of anti-infective agent or anticoagulant, and then wash it with pure water to fully dry it, and then coat a nano-scale parylene organic polymer film layer on the outermost layer. Achieve antibacterial and anticoagulant functions. In the para-xylene organic polymer film coating process, the key lies in the matching of the coating interface (affects the adhesion). Therefore, before the para-xylene organic polymer film is coated with the intravascular catheter, it must be applied first. After the surface of the intravascular catheter is clean, a coupling layer (adhesive layer) must be applied afterwards to increase the adhesion between the intravascular catheter and the parylene organic polymer film, so as to prevent the deposition of intracellular catheters. The toluene organic polymer film (thin film layer) is affected by specific external forces (puncture, friction of intravascular catheters in the body when the human body moves), which causes the film layer to fall off and fail, or cause problems such as thrombosis.

In the above-mentioned conventional manufacturing process, an intravascular catheter is used as a substrate, and the surface of the intravascular catheter is evenly coated with an anti-infective agent or an anticoagulant, and then washed with pure water and dried sufficiently. The meter-level parylene organic polymer thin film layer is not the most enhanced configuration method to achieve the antibacterial and anticoagulant efficacy of intravascular catheters.

In order to avoid the defects of the above-mentioned prior art and strengthen the antibacterial and anticoagulant effects, the present invention uses plasma technology or prior to the vapor deposition (coating) of the parylene organic polymer film (film layer) and the intravascular catheter. The activation solvent serves as an interface activation, which can more effectively improve the adhesion between the parylene organic polymer film (film layer) and the intravascular catheter.

In addition, compared with other high-temperature treatment methods, the plasma technology used in the present invention can make the intravascular catheter less heated (less than 100 degrees), so it is more suitable for intravascular catheter products.

In addition, the present invention completes the coupling layer and coating layer of the intravascular catheter in a vacuum vapor deposition manner, which is different from the metal sputtering process and does not have a directional obstacle, so that the surface of the intravascular catheter can be completely parylene. The organic polymer is tightly covered, thereby forming a transparent film (thin film layer) without pinholes, fine uniformity, high adhesion and high quality.

The parylene organic polymer film coating process of the intravascular catheter of the present invention includes the following steps: cleaning the intravascular catheter, and the step of cleaning the intravascular catheter is selected from one of the following steps: selecting a suitable one for the The pure water of the intravascular catheter is cleaned and fully dried; or the intravascular catheter is placed in the cabin of a batch type plasma vacuum coating equipment, and at least one parameter suitable for the material of the intravascular catheter is selected and injected into the The material of the intravascular catheter matches one of the gases to the chamber of the batch type plasma vacuum coating equipment, and applies plasma technology to excite the gas in the chamber that is evacuated to generate ions and electrons. The ions And impact-peel the surface of the intravascular catheter (to complete the surface cleaning of the intravascular catheter); forming a coupling layer to the surface of the intravascular catheter, and the step of forming a coupling layer to the surface of the intravascular catheter is selected from One of the following steps: choose an infusion solution suitable for the intravascular catheter and dry the intravascular catheter after surface activation; or Use the at least one parameter suitable for the material of the intravascular catheter and inject a gas matching the material of the intravascular catheter into the chamber of the batch type plasma vacuum coating equipment, and apply the plasma technology to the intravascular catheter again And add active particles for vapor deposition (to complete surface activation); place the intravascular catheter in a cabin of a parylene organic polymer vacuum coating equipment and evacuate; and select a suitable intravascular catheter Performance requirements of the at least one parameter One of the performance requirements of intravascular catheters is one of the parylene organic polymer material N type (N TYPE) in a material room. After 120 ~ 150 ℃ vaporization and 650 ~ 800 ℃ cracking zone cracking, it enters about 25 ~ In a normal-temperature deposition chamber at 30 ° C, a uniform nano-scale parylene organic polymer film is formed in the pores on the surface of the intravascular catheter in a vacuum state by vapor deposition.

Therefore, by the above method, the adhesion between the parylene organic polymer film and the intravascular catheter can be surely improved, and the nano-grade parylene organic polymer film can be more tightly and uniformly coated. For purposes within the pores of the surface of an intravascular catheter.

In order to strengthen the antibacterial and anticoagulant effect of the intravascular catheter, a process can be added as required, that is, the intravascular catheter is placed in an infusion solution made of anti-infective or anticoagulant, and the temperature of the immersion liquid is set at 18 ~ Soak at 25 ° C for 10 ~ 60 minutes, and rinse thoroughly with pure water before drying.

The at least one parameter mentioned above is selected from at least one of the following groups: the amount of input gas, the plasma power, and the time value.

The amount of the input gas is between 20 sccm and 200 sccm.

The plasma power is between 100W and 5000W.

The time value mentioned above is between 1 minute and 30 minutes.

The N-type parylene organic polymer material has a film thickness of 0.1 μm to 3 μm.

After the step of forming a uniform parylene organic polymer film in the pores on the surface of the intravascular catheter, the method further includes the following steps: The clean gas breaks the vacuum state of the normal temperature deposition chamber, releases the pressure, and removes the intravascular catheter.

The clean gas system described above is selected from one of the following groups: atmosphere, clean dry gas, and nitrogen.

The anti-infective agent mentioned above refers to rifampicin and / or furacillin.

The anticoagulant mentioned above refers to heparin sodium and the like.

The soaking solution is prepared from an activated solvent Silquest A174 Silane and a medicinal alcohol.

1‧‧‧Intravascular catheter

11‧‧‧ surface

2‧‧‧ batch type plasma vacuum coating equipment

21‧‧‧ cabin

3‧‧‧Polyparaxyl organic polymer vacuum coating equipment

31‧‧‧cabin

32‧‧‧Materials Room

33‧‧‧ Deposition chamber

34‧‧‧ Cracking zone

Steps S1 ~ S4‧‧‧‧

FIG. 1 is a flowchart of a preferred embodiment of the present invention.

FIG. 2 is a perspective view of an intravascular catheter according to a preferred embodiment of the present invention.

FIG. 3 is a schematic diagram of a soaking solution according to a preferred embodiment of the present invention.

FIG. 4 is a schematic diagram of a batch type plasma vacuum coating equipment according to a preferred embodiment of the present invention.

FIG. 5 is a schematic diagram of a parylene organic polymer vacuum coating equipment according to a preferred embodiment of the present invention.

FIG. 6 is a schematic diagram of a coating film cross section of a preferred embodiment of the present invention.

Please refer to FIG. 1, which is a flowchart of a preferred embodiment of the present invention. In FIG. 1, a parylene organic polymer film coating having an intravascular catheter is shown. Process.

Please refer to FIG. 2 to FIG. 6 at the same time, wherein FIG. 2 is a perspective view of the intravascular catheter in the preferred embodiment of the present invention, FIG. 3 is a schematic view of the soaking solution in the preferred embodiment of the present invention, and FIG. 4 is A schematic diagram of a batch type plasma vacuum coating equipment of a preferred embodiment of the present invention, FIG. 5 is a schematic diagram of a parylene organic polymer vacuum coating equipment of a preferred embodiment of the present invention, and FIG. 6 is a comparison of the present invention. A schematic diagram of the coating film cross section of the preferred embodiment. Please refer to FIG. 1 together.

As shown in the figure, the poly-para-xylylene organic polymer film coating process of the intravascular catheter 1 (as shown in FIG. 2) is to first clean the intravascular catheter 1 (step S1).

The above steps for cleaning the intravascular catheter 1 may be selected from one of the following steps: pure water suitable for the intravascular catheter 1 is washed and dried sufficiently; or the intravascular catheter 1 is placed in a batch type plasma vacuum coating equipment 2 of the tank 21 (as shown in FIG. 4); select at least one parameter suitable for the material of the intravascular catheter 1 and inject a gas matching the material of the intravascular catheter 1 into the batch plasma vacuum coating equipment 2 The chamber 21 is evacuated, and plasma technology is applied to excite the gas in the evacuated chamber 21 to generate ions and electrons. The ions impact and erode the surface 11 of the intravascular catheter 1. With this step, the surface 11 of the intravascular catheter 1 can be cleaned. (Note: The aforementioned batch-type plasma vacuum coating equipment may be a batch-type plasma vacuum coating equipment developed by one of the applicants (Lach Company)).

The at least one parameter mentioned above may be selected from at least one of the following groups: the amount of input gas, the plasma power, and the time value. The aforementioned amount of input gas can be between 20ccm (the flow rate unit controlled by the mass flow controller (MFC)) to 200cm; plasma power can be between 100W and 5000W; time value (process time value) can be between 1 minute To 30 minutes.

In the embodiment shown in the above step S1, the plasma power is selected from 500W ~ 5000W energy, and the time value is selected from 1 ~ 30 minutes. In addition, the gas system matching the material of the intravascular catheter 1 can be selected from various gases, such as air, oxygen, argon, a mixture of argon and hydrogen, a mixture of tetrafluoromethane and oxygen, and the like.

Through the above step S1, the AC and DC electric fields free atoms and molecules. This plasma technology is an inelastic collision. An electron collides with a neutral atom and a molecule to form a positive ion and two free electrons. These two electrons are obtained from the electric field. After energy, more electrons and ions are produced through free collision, forming a plasma discharge. Electron collision excites the gas in the chamber 21 in a vacuum state, generating ions and electrons, and eroding the surface 11 of the intravascular catheter 1 through the impact of the ions, which can complete the cleanliness requirements of the surface 11 of the intravascular catheter 1 and increase the intravascular catheter 1 Surface roughness.

Thereafter, a coupling layer (as shown in FIG. 6, which can also be referred to as an adhesion layer) is formed on the surface 11 of the intravascular catheter 1 (step S2).

The above-mentioned step of forming a coupling layer to the surface 11 of the intravascular catheter 1 may be selected from one of the following steps: selecting an infusion solution (activating solvent) suitable for the intravascular catheter, for example, an activating solvent Silquest A174 Silane and an Medicinal alcohol is prepared (as shown in Figure 3), and the surface 11 of the intravascular catheter 1 is fully dried after activation; or at least one parameter suitable for the material of the intravascular catheter 1 is selected and injected into the material of the intravascular catheter 1 Match one gas to the chamber 21 of the batch type plasma vacuum coating equipment 2, and then Plasma technology was applied to the intravascular catheter 1 once, and active particles were added for vapor deposition. With this step, activation of the surface 11 of the intravascular catheter 1 can be completed.

In the embodiment shown in the above step S2, according to the adhesion requirement of the intravascular catheter 1, for example, a plasma power of 100W ~ 5000W energy, a time value of 1 ~ 20 minutes, and a gas (such as air, Oxygen, argon, argon-hydrogen mixed gas, tetrafluoromethane and oxygen mixed gas, etc.) into the chamber 21 of the batch type plasma vacuum coating equipment 2, and for the chamber 21 of the batch type plasma vacuum coating equipment 2 The intravascular catheter 1 is again subjected to plasma technology, and active particles are added (for example, organosilicon compounds, such as hexamethyldisilazane, hexamethyldisilazane, silane, azasilane, fluorine-containing chemicals, etc.) Vapor deposition is performed to meet the requirements for effective modification of the surface 11 of the intravascular catheter 1, and to increase the adhesion between the intravascular catheter 1 and the parylene organic polymer film.

Then, the intravascular catheter 1 is placed in a chamber 31 (shown in FIG. 5) of a parylene organic polymer vacuum coating device 3 and evacuated (step S3). (Note: The aforementioned parylene organic polymer vacuum coating equipment can be a parylene organic polymer vacuum coating equipment independently developed by one of the applicants (Lach Company)).

Then, at least one parameter suitable for the performance requirement of the intravascular catheter 1 is selected and injected into a material chamber 32 with a parylene organic polymer material N-type that matches the performance requirement of the intravascular catheter 1. After vaporization at 120 ~ 150 ℃ and cracking in 650 ~ 800 ℃ cracking zone 34, it enters into a normal temperature deposition chamber 33 at about 25 ~ 30 ℃, and forms a uniform conglomerate by vapor deposition under vacuum. The xylene organic polymer film is in the pores of the surface 11 of the intravascular catheter 1 (step S4).

In the embodiment shown in step S4 above, according to the material of the intravascular catheter 1, suitable para-xylene organic polymer material N-TYPE is selected with suitable coating parameters, and the para-xylene organic polymer material is put into In the material chamber 32, after vaporization at 120-150 ° C and cracking in the 650-800 ° C cracking zone 34, the solid bivalent polymer is vaporized and cracked into monovalent nano-scale organic polymer gas, and then introduced into about 25-30 Vapor deposition is performed in a normal-temperature deposition chamber 33 at a temperature of 0 ° C. Please refer to Figure 6 for a schematic diagram of the coating section after the coating is completed.

The thickness of the above-mentioned parylene organic polymer film can be set to 0.1 μm to 3 μm according to requirements. In addition, the above-mentioned parylene organic polymer vacuum coating equipment 3 may be designed with a pressure-controlling and baffle plate (not shown). The uniform and stable deposition causes the surface 11 of the intravascular catheter 1 to form a highly uniform, highly transparent film (film layer).

After the embodiment shown in the above step S4, a process can be added as required, that is, the intravascular catheter 1 is placed in an infusion solution made of an anti-infective agent or an anticoagulant. The temperature of the immersion liquid is set at 18 ~ 25 ° C, and the immersion is performed. After 10 to 60 minutes, rinse with pure water and fully dry, as shown in Figure 6, which can further strengthen the antibacterial and anticoagulant effects of the intravascular catheter 1.

Therefore, by the above method, the adhesion between the parylene organic polymer film and the intravascular catheter can be surely improved, and the nano-grade parylene organic polymer film can be more tightly and uniformly wrapped. The purpose of covering the pores on the surface of the intravascular catheter achieves nano-grade hydrophobic membrane quality. After that, it can be coated with anti-infective or anticoagulant on the outer layer according to the different needs of the intravascular catheter. Antibacterial and anticoagulant effect of intravascular catheter.

In addition, in the above-mentioned parylene organic polymer film coating process, after the step of forming a uniform parylene organic polymer film in the pores of the surface 11 of the intravascular catheter 1, the method may further include the following steps: The vacuum state of the normal temperature deposition chamber 33 is broken with a clean gas, the pressure is released, and the intravascular catheter 1 is taken out.

The above clean gas may be selected from one of the following groups: atmosphere, clean dry gas, and nitrogen.

After the above parylene organic polymer thin film coating process, other processes can be performed, such as using a thin film measuring instrument to measure the thickness of the parylene organic polymer thin film, or according to the required performance of the intravascular catheter 1. If required, perform a hydrophobicity measurement test.

The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, and improvements made within the spirit and principle of the present invention should be included in the present invention. Within the scope of protection.

Claims (8)

A polyparaxylene organic polymer film coating process for an intravascular catheter includes the following steps: cleaning the intravascular catheter, and the step of cleaning the intravascular catheter is selected from one of the following steps: selecting a suitable one for the blood vessel The pure water in the inner catheter is cleaned and fully dried; or the inner catheter is placed in the cabin of a batch type plasma vacuum coating equipment, and at least one parameter suitable for the material of the inner catheter is selected and injected into the vessel. The material of the inner tube matches one of the gases into the chamber of the batch-type plasma vacuum coating equipment and evacuates it, and applies plasma technology to excite the gas in the evacuated chamber to generate ions and electrons. The ion impacts and erodes the surface of the intravascular catheter; forming a coupling layer to the surface of the intravascular catheter, and the step of forming a coupling layer to the surface of the intravascular catheter is selected from one of the following steps: Suitable for an infusion solution of the intravascular catheter, which is sufficiently dried after surface activation of the intravascular catheter; The at least one parameter of the quality and inject a gas that matches the material of the intravascular catheter into the chamber of the batch type plasma vacuum coating equipment, apply plasma technology to the intravascular catheter again, and add active particles Performing vapor deposition; placing the intravascular catheter in a chamber of a parylene organic polymer vacuum coating equipment and evacuating the vacuum; and selecting the at least one parameter suitable for the performance requirements of the intravascular catheter and injecting the The performance requirements of the intravascular catheter match one of the para-paraxyl organic polymer materials N-type in a material chamber. After vaporization at 120 ~ 150 ° C and cracking in the 650 ~ 800 ° C cracking zone, it enters about 25 ~ 30 ° C. In a normal temperature deposition chamber, under vacuum, a uniform parylene organic polymer film is formed in the pores on the surface of the intravascular catheter by vapor deposition; wherein the at least one parameter is selected from the following group At least one of the groups: the amount of gas input, plasma power and time value. According to the para-xylene organic polymer film coating process of the intravascular catheter described in the first patent application scope, the amount of input gas is between 20 sccm and 200 sccm. According to the para-xylene organic polymer thin film coating process of the intravascular catheter described in the first patent application scope, the plasma power is between 100W and 5000W. The process for coating a polyparaxylene organic polymer film of an intravascular catheter according to item 1 of the scope of patent application, wherein the time value is between 1 minute and 30 minutes. According to the process for coating a polyparaxylene organic polymer film of an intravascular catheter according to item 1 of the scope of application for a patent, the thickness of the parylene organic polymer film is 0.1 μm to 3 μm. The process for coating a polyparaxylene organic polymer film of an intravascular catheter according to item 1 of the scope of application for a patent, wherein a uniform parylene organic polymer film is formed in the pores on the surface of the intravascular catheter. After the step, the method further includes the steps of breaking the vacuum state of the normal-temperature deposition chamber with a clean gas, releasing the pressure, and removing the intravascular catheter. According to the process of coating a polyparaxylylene organic polymer thin film for an intravascular catheter as described in item 6 of the scope of patent application, the clean gas system is selected from one of the following groups: atmosphere, clean dry gas, and nitrogen. The para-xylene organic polymer film coating process for the intravascular catheter according to item 1 of the patent application scope, wherein the soaking solution is prepared from an activated solvent Silquest A174 Silane and a medicinal alcohol.