CN209854235U

CN209854235U - Separation type vacuum coating pipe fitting

Info

Publication number: CN209854235U
Application number: CN201920588455.8U
Authority: CN
Inventors: 孙建军
Original assignee: Individual
Current assignee: Individual
Priority date: 2019-04-27
Filing date: 2019-04-27
Publication date: 2019-12-27
Anticipated expiration: 2029-04-27

Abstract

The utility model discloses a separation type vacuum coating pipe fitting, including the plastic tubing, the inboard deposit of pipe wall of plastic tubing has the SiO film, and the SiO film outside deposit has the SiO film₂A film; SiO thin film and SiO are deposited on the outer side of the pipe wall from inside to outside in sequence₂Films and silicon nitride films. The utility model adopts the vacuum coating (PECVD, PVD) method to carry out on the inner wall and the outer wall of the PET, PEN and other plastic pipesLow speed SiO and high speed SiO₂The film is deposited, so that microscopic pores on the surface of the plastic pipe are filled, and water vapor molecules, oxygen molecules and carbon dioxide molecules are not easy to permeate into the inner wall of the pipe to influence the test accuracy of the sample; in addition, the utility model utilizes low-speed SiO and high-speed SiO₂The combined mode improves the compactness of the barrier film and prolongs the penetration distance, and simultaneously utilizes the silicon nitride to form SiO on the surface of the outer wall₂The modification is carried out, and the hydrophilic property is changed into the hydrophobic property, so that the influence of water stain and dirt is avoided.

Description

Separation type vacuum coating pipe fitting

Technical Field

The utility model relates to a vacuum coating field especially relates to a separation type vacuum coating pipe fitting.

Background

At present, plastic pipe fittings are mostly made of materials such as PET and PEN, the plastic pipe fittings are light in weight, convenient to transport and small in damage probability, however, compared with glass pipes, the plastic pipes are high in water vapor permeability, and long-term storage easily causes related index variation of analysis samples in the pipes, for example, PET pipes/bottles are formed by injection molding processing of bottle blanks and are formed by blow molding processing again, the plastic pipe fittings have high hygroscopicity, the water absorption rate is 0.6%, and water molecules absorbed by the PET pipes/bottles can block the formation of gas barrier films, so that the barrier performance of the film layers is reduced.

In order to solve the problems, the conventional method is to isolate various interference sources such as water vapor, oxygen, carbon dioxide and the like by using a method of thickening the pipe wall by using a double-layer pipe, but the relatively thorough water and oxygen isolation effect cannot be realized, the transparency of the pipe fitting is influenced, and the production cost is increased.

SUMMERY OF THE UTILITY MODEL

To the deficiency of prior art, the utility model provides a separation type vacuum coating pipe fitting, the utility model discloses a vacuum coating (PECVD, PVD) method carries out low-speed SiO and high-speed SiO at plastics pipe fittings inner wall and outer wall such as PET, PEN₂And the film is deposited, so that the isolation effect of water vapor, oxygen and carbon dioxide is improved. Simultaneously SiO on the outer wall of the pipe fitting₂The hydrophobic layer film silicon nitride is continuously deposited on the film, so that the problems of water stain, dirt and the like possibly occurring on the outer wall are avoided, and the purpose of further protecting the in-tube analysis sample is achieved.

The technical scheme of the utility model as follows: a barrier type vacuum coating pipe fitting comprises a plastic pipe, wherein a SiO thin film and a SiO film are sequentially deposited on the inner side of the pipe wall of the plastic pipe₂A film; the outer side of the pipe wall of the plastic pipe is sequentially deposited with a SiO film and SiO from inside to outside₂Films and silicon nitride films.

Preferably, the plastic pipe is made of PET, PEN, PP or COP materials, the length of the plastic pipe is 30-1500 mm, the outer diameter of the plastic pipe is 30-1000 mm, and the thickness of the plastic pipe is 1-10 mm. Preferably, the length of the plastic pipe is 30-500 mm, the outer diameter of the plastic pipe is 30-100 mm, and the thickness of the plastic pipe is 1-5 mm.

Preferably, the SiO thin film deposited on the inner side of the tube wall is a low-speed deposition film deposited by a PECVD method, the thickness is 5-10 nm, the deposition time is 15-30 seconds, and SiO is deposited on the inner side of the tube wall₂The film is a high-speed deposition film and is deposited by a PECVD method, the thickness of the film is 20-70 nm, and the film is depositedThe time is 30-105 seconds.

Preferably, the SiO thin film deposited on the outer side of the tube wall is a low-speed deposition film and is deposited by adopting a PVD method, the thickness is 1-5 nm, the deposition time is 120-600 seconds, and SiO is deposited₂The film is a high-speed deposition film and is deposited by a PVD method, the thickness of the film is 5-10 nm, the deposition time is 60-300 seconds, and the silicon nitride film is deposited by the PVD method, the thickness of the film is 5-10 nm, and the deposition time is 60-120 seconds.

The utility model has the characteristics as follows: the utility model discloses utilize the PECVD technique of normal atmospheric temperature to realize the pipe fitting inner wall coating film of high draw ratio. Meanwhile, a CCP discharge gas input method and an inductively coupled ICP discharge method are combined to generate high-density plasma in the pipe fitting, and a coil is used for generating a magnetic field to enhance discharge strength, so that ionized gas in the pipe fitting is uniformly distributed to ensure the uniformity and stability of film deposition. The low-speed SiO deposited on the inner wall and the outer wall of the plastic pipe/bottle has the advantages that the deposition speed is low, the film is compact, the surface defects are few, and the separation effect of influence sources such as water vapor and the like is easy to promote; high-speed SiO deposited on inner wall and outer wall₂The layer can increase the thickness of the barrier layer as a whole, so that water vapor molecules, oxygen molecules and carbon dioxide molecules have to traverse a longer path and take longer time to permeate into the pipe, thereby indirectly prolonging the storage time of the sample. In addition, the silicon nitride film deposited on the outer wall has hydrophobic effect, and SiO have hydrophobic effect₂The plastic tube/bottle is a hydrophilic film, so that the hydrophilic layer exposed on the outermost surface is modified into a hydrophobic layer, and the outer surface of the plastic tube/bottle is not easily polluted by water and dirt. The multilayer film composite structure can greatly improve the barrier property of the plastic pipe to water vapor and oxygen, can be widely applied to a plurality of fields of medicine packaging, food packaging, flexible period packaging and the like, and has the advantages of relatively simple manufacturing process, lower cost and no pollution to the environment.

Compared with the prior art, the utility model discloses following beneficial effect has: the utility model fills microscopic pores on the surface of plastic pipes such as PET, PEN and the like, and water vapor molecules, oxygen molecules and carbon dioxide molecules are not easy to permeate into the inner wall of the pipe to influence the test accuracy of the sample; in addition, the first and second substrates are,the utility model utilizes low-speed SiO and high-speed SiO₂The combined mode improves the compactness of the barrier film and prolongs the penetration distance, and simultaneously utilizes the silicon nitride to form SiO on the surface of the outer wall₂The modification is carried out, and the hydrophilic property is changed into the hydrophobic property, so that the influence of water stain and dirt is avoided.

Drawings

Fig. 1 is a sectional view of a coating film of the barrier type pipe fitting provided by the present invention;

the labels in the figure are: 1-tube wall, 2-first SiO film, 3-first SiO₂Film, 4-second SiO film, 5-second SiO₂Film, 6-silicon nitride film.

Detailed Description

The technical solutions of the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments, but the present invention is not limited to the following technical solutions.

Example 1

At present, the sodium citrate vacuum blood collection tube with large medical market consumption is made of PET plastic, and a first SiO (silicon monoxide) film 2 with the thickness of 10nm is deposited on the inner side of a tube wall 1 at a low speed; high-speed deposition of 70nm first SiO (silicon monoxide) on the outer side of the first SiO film₂(silica) film 3; depositing a second SiO (silicon monoxide) film 4 with the thickness of 5nm at low speed on the outer side of the tube wall, and then depositing a second SiO (silicon monoxide) film with the thickness of 10nm at high speed₂A (silicon dioxide) film 5 and finally a 10nm silicon nitride film 6 is deposited as a hydrophobic layer structure as shown in figure 1.

The method comprises the following specific steps of:

selecting a PET (polyethylene terephthalate) sodium citrate blood collection tube with the length of 75mm, the outer diameter of the tube of 10mm and the wall thickness of the tube of 1mm as a base material, soaking the blood collection tube in 95% ethanol, ultrasonically cleaning for 5 minutes, blow-drying by using nitrogen, removing static electricity by using a surface static gun, immediately putting the blood collection tube into a vacuum coating chamber, wherein the vacuum coating chamber is internally provided with a thimble-shaped Pin structure for supporting the inner wall of a tube and ensuring that the tube is stably fixed in the coating chamber. Then the coating chamber is vacuumized to 1.97Pa, oxygen or argon of 50sccm is introduced for 5 minutes, and oxygen or argon plasma is utilized to enter the inner wall and the outer wall of the pipe fittingThe line surface is bombarded to improve the surface energy of the surface of the pipe fitting, which is beneficial to improving the adhesive force of the subsequent SiO deposition film layer. After the oxygen or argon ion bombardment is finished, introducing silane gas and oxygen gas, keeping the air pressure at 5-15.7 Pa, generating high-density plasma in the pipe fitting by combining a CCP discharge gas input method and an inductively coupled ICP discharge method under the conditions of room temperature of 25 ℃, discharge power of 50W and the like, and generating a magnetic field by using a coil to enhance the discharge strength so that ionized gas in the pipe fitting is uniformly distributed to ensure the uniformity and stability of film deposition. The low-speed SiO with the thickness of about 10nm is deposited according to the experimental method, and the deposition time is about 30 seconds. Then changing the discharge power to 100W, keeping the air pressure at 10-19.7 Pa, depositing the inside of the pipe for about 105 seconds by the same method to prepare SiO with the thickness of 70nm₂. And finishing the coating of the inner wall of the pipe fitting.

Then, by using the PVD magnetron sputtering technology, Ar with the purity of 99.999 percent of 200sccm and O with the purity of 1000sccm are introduced under the conditions of 50W and 100W of power₂Keeping the air pressure at 0.1-1.0 Pa, controlling Ar ions to bombard the Si target material through a magnetic field, and respectively depositing low-speed SiO with the thickness of 1-5 nm and high-speed SiO with the thickness of 5-10 nm₂Then, by switching gas sources, O is added₂Replacing the solution with N with the purity of 99.999 percent and the flow rate of 1400sccm₂The power is adjusted to 250W, the deposition time is controlled to be about 60 seconds, and the Ar ions are controlled by the magnetic field to bombard the Si target material to continuously deposit silicon nitride with the thickness of 5 nm.

The structure of the coated pipe obtained in example 1 is shown in fig. 1, and when the barrier effect of the coated pipe is determined, the permeability of interference sources such as water vapor molecules, oxygen molecules and carbon dioxide molecules can be reduced from 0.002g/Pkg 24h to 0.0002g/Pkg 24h, and the barrier capability is improved by about 10 times. The test accuracy of the medical sample after long-term storage can be ensured.

Example 2

In the food packaging industry, for example, liquid substances in plastic bottles such as PET (polyethylene terephthalate), PEN, PP or COP (polyethylene terephthalate), and the like in beer, beverages and the like are stored after the inner wall and the outer wall are subjected to vacuum coating treatment by adopting the design, and the storage time can be prolonged from 1 month to more than 4 months conventionally. The method comprises the following specific steps:

the PET bottle with the volume of 2L is selected as a base material, the bottle is soaked in 95% ethanol and cleaned by ultrasonic waves for 5 minutes, then the bottle is dried by using nitrogen and subjected to static electricity removal by using a surface static gun, and then the bottle is immediately placed into a vacuum coating chamber, wherein the vacuum coating chamber is internally provided with a needle-shaped Pin structure for supporting the inner wall of the bottle and ensuring that the bottle is stably fixed in the coating chamber. And then the coating chamber is vacuumized to 1.97Pa, 50sccm oxygen or argon is introduced for 5 minutes, and oxygen or argon plasma is utilized to carry out surface bombardment on the inner wall and the outer wall of the bottle so as to improve the surface energy of the surface of the pipe fitting and be beneficial to improving the adhesive force of a subsequent SiO deposition film layer. After the oxygen or argon ion bombardment is finished, introducing silane gas and oxygen gas, keeping the air pressure at 5-15.7 Pa, generating high-density plasma in the bottle by combining a CCP discharge gas input method and an inductively coupled ICP discharge method under the conditions of room temperature of 25 ℃, discharge power of 50W and the like, and generating a magnetic field by using a coil to enhance the discharge intensity so that ionized gas in the bottle is uniformly distributed to ensure the uniformity and stability of film deposition. The low-speed SiO with the thickness of about 10nm is deposited according to the experimental method, and the deposition time is about 30 seconds. Then changing the discharge power to 100W, keeping the air pressure at 10-19.7 Pa, depositing the inside of the pipe for about 105 seconds by the same method to prepare SiO with the thickness of 70nm₂. And finishing the coating of the inner wall of the pipe fitting. Then, by using the PVD magnetron sputtering technology, Ar with the purity of 99.999 percent of 200sccm and O with the purity of 1000sccm are introduced under the conditions of 50W and 100W of power₂Keeping the air pressure at 0.1-1.0 Pa, controlling Ar ions to bombard the Si target material through a magnetic field, and respectively depositing low-speed SiO with the thickness of 3nm and high-speed SiO with the thickness of 7nm₂Then, by switching gas sources, O is added₂Replacing the solution with N with the purity of 99.999 percent and the flow rate of 1400sccm₂The power is adjusted to 250W, the deposition time is controlled to be about 120 seconds, and the Ar ions are controlled by the magnetic field to bombard the Si target material to continuously deposit silicon nitride with the thickness of 10 nm.

The coating method does not affect the appearance design and transparency of the PET bottle, the total thickness of the coating is 100nm, and the shelf life of the beer bottled in the PET bottle can reach 4-12 months.

Claims

1. A barrier type vacuum coating pipe fitting comprises a plastic pipe and is characterized in that a SiO film and a SiO film are sequentially deposited on the inner side of the pipe wall of the plastic pipe₂A film; the outer side of the pipe wall of the plastic pipe is sequentially deposited with a SiO film and SiO from inside to outside₂Films and silicon nitride films.

2. The barrier vacuum coated pipe as claimed in claim 1, wherein the plastic pipe is made of PET, PEN, PP or COP, and has a length of 30-1500 mm, an outer diameter of 30-1000 mm and a thickness of 1-10 mm.

3. The barrier vacuum coated pipe as claimed in claim 1, wherein the SiO thin film deposited on the inner side of the pipe wall is a low-speed deposited film deposited by PECVD method with thickness of 5-10 nm and deposition time of 15-30 s, and SiO is deposited on the inner side of the pipe wall₂The film is a high-speed deposition film and is deposited by a PECVD method, the thickness is 20-70 nm, and the deposition time is 30-105 seconds.

4. The barrier vacuum coated pipe as claimed in claim 1, wherein the SiO thin film deposited on the outer side of the pipe wall is a low-speed deposited film deposited by PVD method with thickness of 1-5 nm and deposition time of 120-600 s, and SiO thin film is deposited by PVD method with thickness of 1-5 nm and deposition time of 120-600 s₂The film is a high-speed deposition film and is deposited by a PVD method, the thickness of the film is 5-10 nm, the deposition time is 60-300 seconds, and the silicon nitride film is deposited by the PVD method, the thickness of the film is 5-10 nm, and the deposition time is 60-120 seconds.