A shaped hose inner wall coating for choledochoscope and preparation method thereof

Abstract

A coating for the inner wall of a shaped hose for a choledochoscope and a preparation method thereof. In order to improve the wear resistance of the inner wall of the shaped hose for a choledochoscope and to make it have a suitable fatigue life, the MoS2 soft coating prepared by the present invention can effectively improve the wear resistance of the material, and by adding Nb to the MoS2 soft coating, its fatigue life can be effectively improved. However, the addition of Nb will cause the wear resistance of the MoS2 soft coating to decrease, so the mass content of Nb in the coating needs to be controlled at 9wt%-22wt% to meet the use requirements of medical materials.

Description

Technical Field

[0001] The invention relates to the field of medical coatings for a shaped hose for a choledochoscope, and in particular to an inner wall coating for a shaped hose for a choledochoscope and a preparation method thereof. Background Art

[0002] During biliary surgery, choledochoscopes can provide more information about the bile duct system, such as whether there are stones, stenosis, or tumors in the common bile duct and intrahepatic bile duct, and whether the lower segment of the common bile duct is unobstructed. Choledochoscopes are divided into rigid and flexible types. Rigid endoscopes can only observe the common bile duct, while flexible endoscopes can deliver the endoscope to the 2nd to 3rd level hepatic ducts, so flexible choledochoscopes are often used. The shaped hose adjusts the bending angle according to the observation results of the laparoscope, forming a surgical channel between the common bile duct and the outside of the human body for the choledochoscope to enter the common bile duct through the surgical channel to remove stones.

[0003] However, due to the contact friction between the choledochoscope and the shaping hose, the choledochoscope and the shaping hose are worn to varying degrees, thereby shortening their service life. On the other hand, fatigue damage to the shaping hose during long-term bending is also a problem that cannot be ignored. Therefore, it is necessary to design a shaping hose that is wear-resistant and has a long fatigue life. Summary of the invention

[0004] In view of the problems existing in the prior art, the purpose of the present invention is to provide a method for preparing the inner wall coating of a shaped hose for a choledochoscope, by which a MoS2-Nb soft composite coating whose wear resistance and fatigue strength meet the use requirements of the shaped hose for a choledochoscope can be obtained.

[0005] A method for preparing an inner wall coating of a shaped hose for a choledochoscope, characterized in that the preparation method comprises the following steps:

[0006] The metal choledochoscope shaping hose is placed in a mixed solution of acetic acid and HCl for polishing; the polished shaping hose is placed in a mixed solution of sodium carbonate and OP-10 emulsifier for degreasing; the degreasing shaping hose is ultrasonically cleaned with deionized water until there is no residual agent on the inner wall, and finally dried;

[0007] The shaped hose is placed in a sputtering coating machine, and a cylindrical target is selected to coat the inner wall of the shaped hose with a MoS2-Nb soft wear-resistant coating, wherein the target is a MoS2-Nb composite target (the mass content of Nb is 9wt%-22wt%), and the sputtering process uses argon as the working gas, the sputtering pressure is 8Pa, the sputtering temperature is 120°C, the argon flow rate is 80sccm, and the sputtering time is 45min;

[0008] The shaped hose coated with the MoS2-Nb soft coating is placed in a vacuum annealing furnace for low-temperature annealing, the annealing temperature is 180-200°C, and the annealing time is 1.5-2.0h.

[0009] Preferably, the concentration of the acetic acid is 20%.

[0010] Preferably, the concentration of HCl is 10%.

[0011] Preferably, the concentration of sodium carbonate is 22%.

[0012] Preferably, the concentration of the OP-10 emulsifier is 8%.

[0013] Preferably, the drying process is performed under a nitrogen atmosphere.

[0014] Furthermore, the present invention also provides a coating for the inner wall of a shaped hose for a choledochoscope, and the coating is prepared by the above method.

[0015] In order to improve the wear resistance of the inner wall of the shaped hose for choledochoscope and make it have a suitable fatigue life, the MoS2 soft coating prepared by the present invention can effectively improve the wear resistance of the material, and by adding Nb to the MoS2 soft coating, its fatigue life can be effectively improved. However, the addition of Nb will cause the wear resistance of the MoS2 soft coating to decrease. Therefore, the mass content of Nb in the coating needs to be controlled at 9wt%-22wt% to meet the use requirements of medical materials. DETAILED DESCRIPTION

[0016] The technical effects of the present invention are verified below through specific examples, but the embodiments of the present invention are not limited thereto.

[0017] Example 1

[0018] The metal choledochoscope shaping hose was placed in a mixed solution of acetic acid and HCl for polishing, wherein the concentration of acetic acid in the polishing solution was 20% and the concentration of HCl was 10%. The polished shaping hose was placed in a mixed solution of sodium carbonate and OP-10 emulsifier for degreasing, wherein the concentration of sodium carbonate in the degreasing agent was 22% and the concentration of OP-10 emulsifier was 8%. The degreasing shaping hose was ultrasonically cleaned with deionized water until there was no residual agent on the inner wall, and finally dried in a nitrogen atmosphere.

[0019] The shaped hose is placed in a sputtering coating machine, and a cylindrical target is used to coat the inner wall of the shaped hose with a soft wear-resistant coating. The target is a MoS2-9wt% Nb composite target. Argon is used as the working gas in the sputtering process, the sputtering pressure is 8Pa, the sputtering temperature is 120°C, the argon flow rate is 80sccm, and the sputtering time is 45min.

[0020] The shaped hose coated with the MoS2-Nb soft coating was placed in a vacuum annealing furnace for low temperature annealing. The annealing temperature was 200°C and the annealing time was 1.5 h.

[0021] Example 2

[0022] The metal choledochoscope shaping hose was placed in a mixed solution of acetic acid and HCl for polishing, wherein the concentration of acetic acid in the polishing solution was 20% and the concentration of HCl was 10%. The polished shaping hose was placed in a mixed solution of sodium carbonate and OP-10 emulsifier for degreasing, wherein the concentration of sodium carbonate in the degreasing agent was 22% and the concentration of OP-10 emulsifier was 8%. The degreasing shaping hose was ultrasonically cleaned with deionized water until there was no residual agent on the inner wall, and finally dried in a nitrogen atmosphere.

[0023] The shaped hose is placed in a sputtering coating machine, and a cylindrical target is used to coat the inner wall of the shaped hose with a soft wear-resistant coating. The target is a MoS2-12wt% Nb composite target. Argon is used as the working gas in the sputtering process, the sputtering pressure is 8Pa, the sputtering temperature is 120°C, the argon flow rate is 80sccm, and the sputtering time is 45min.

[0024] The shaped hose coated with the MoS2-Nb soft coating was placed in a vacuum annealing furnace for low temperature annealing. The annealing temperature was 200°C and the annealing time was 1.5 h.

[0025] Example 3

[0026] The metal choledochoscope shaping hose was placed in a mixed solution of acetic acid and HCl for polishing, wherein the concentration of acetic acid in the polishing solution was 20% and the concentration of HCl was 10%. The polished shaping hose was placed in a mixed solution of sodium carbonate and OP-10 emulsifier for degreasing, wherein the concentration of sodium carbonate in the degreasing agent was 22% and the concentration of OP-10 emulsifier was 8%. The degreasing shaping hose was ultrasonically cleaned with deionized water until there was no residual agent on the inner wall, and finally dried in a nitrogen atmosphere.

[0027] The shaped hose is placed in a sputtering coating machine, and a cylindrical target is used to coat the inner wall of the shaped hose with a soft wear-resistant coating. The target is a MoS2-15wt% Nb composite target. Argon is used as the working gas in the sputtering process, the sputtering pressure is 8Pa, the sputtering temperature is 120°C, the argon flow rate is 80sccm, and the sputtering time is 45min.

[0028] The shaped hose coated with the MoS2-Nb soft coating was placed in a vacuum annealing furnace for low temperature annealing. The annealing temperature was 200°C and the annealing time was 1.5 h.

[0029] Example 4

[0030] The metal choledochoscope shaping hose was placed in a mixed solution of acetic acid and HCl for polishing, wherein the concentration of acetic acid in the polishing solution was 20% and the concentration of HCl was 10%. The polished shaping hose was placed in a mixed solution of sodium carbonate and OP-10 emulsifier for degreasing, wherein the concentration of sodium carbonate in the degreasing agent was 22% and the concentration of OP-10 emulsifier was 8%. The degreasing shaping hose was ultrasonically cleaned with deionized water until there was no residual agent on the inner wall, and finally dried in a nitrogen atmosphere.

[0031] The shaped hose is placed in a sputtering coating machine, and a cylindrical target is used to coat the inner wall of the shaped hose with a soft wear-resistant coating. The target is a MoS2-17wt% Nb composite target. Argon is used as the working gas in the sputtering process, the sputtering pressure is 8Pa, the sputtering temperature is 120°C, the argon flow rate is 80sccm, and the sputtering time is 45min.

[0032] The shaped hose coated with the MoS2-Nb soft coating was placed in a vacuum annealing furnace for low temperature annealing. The annealing temperature was 200°C and the annealing time was 1.5 h.

[0033] Example 5

[0034] The metal choledochoscope shaping hose was placed in a mixed solution of acetic acid and HCl for polishing, wherein the concentration of acetic acid in the polishing solution was 20% and the concentration of HCl was 10%. The polished shaping hose was placed in a mixed solution of sodium carbonate and OP-10 emulsifier for degreasing, wherein the concentration of sodium carbonate in the degreasing agent was 22% and the concentration of OP-10 emulsifier was 8%. The degreasing shaping hose was ultrasonically cleaned with deionized water until there was no residual agent on the inner wall, and finally dried in a nitrogen atmosphere.

[0035] The shaped hose is placed in a sputtering coating machine, and a cylindrical target is used to coat the inner wall of the shaped hose with a soft wear-resistant coating. The target is a MoS2-22wt% Nb composite target. Argon is used as the working gas in the sputtering process, the sputtering pressure is 8Pa, the sputtering temperature is 120°C, the argon flow rate is 80sccm, and the sputtering time is 45min.

[0036] The shaped hose coated with the MoS2-Nb soft coating was placed in a vacuum annealing furnace for low temperature annealing. The annealing temperature was 200°C and the annealing time was 1.5 h.

[0037] Comparative Example 1

[0038] The metal choledochoscope shaping hose was placed in a mixed solution of acetic acid and HCl for polishing, wherein the concentration of acetic acid in the polishing solution was 20% and the concentration of HCl was 10%. The polished shaping hose was placed in a mixed solution of sodium carbonate and OP-10 emulsifier for degreasing, wherein the concentration of sodium carbonate in the degreasing agent was 22% and the concentration of OP-10 emulsifier was 8%. The degreasing shaping hose was ultrasonically cleaned with deionized water until there was no residual agent on the inner wall, and finally dried in a nitrogen atmosphere.

[0039] The shaped hose is placed in a sputtering coating machine, and a cylindrical target is used to coat the inner wall of the shaped hose with a soft wear-resistant coating. The target material is MoS2 material, and argon is used as the working gas in the sputtering process. The sputtering pressure is 8Pa, the sputtering temperature is 120℃, the argon flow rate is 80sccm, and the sputtering time is 45min.

[0040] The shaped hose coated with the MoS2 soft coating was placed in a vacuum annealing furnace for low temperature annealing. The annealing temperature was 200°C and the annealing time was 1.5 h.

[0041] Comparative Example 2

[0042] The metal choledochoscope shaping hose was placed in a mixed solution of acetic acid and HCl for polishing, wherein the concentration of acetic acid in the polishing solution was 20% and the concentration of HCl was 10%. The polished shaping hose was placed in a mixed solution of sodium carbonate and OP-10 emulsifier for degreasing, wherein the concentration of sodium carbonate in the degreasing agent was 22% and the concentration of OP-10 emulsifier was 8%. The degreasing shaping hose was ultrasonically cleaned with deionized water until there was no residual agent on the inner wall, and finally dried in a nitrogen atmosphere.

[0043] The shaped hose is placed in a sputtering coating machine, and a cylindrical target is used to coat the inner wall of the shaped hose with a soft wear-resistant coating. The target is a MoS2-35wt% Nb composite target. Argon is used as the working gas in the sputtering process, the sputtering pressure is 8Pa, the sputtering temperature is 120°C, the argon flow rate is 80sccm, and the sputtering time is 45min.

[0044] The shaped hose coated with the MoS2-Nb soft coating was placed in a vacuum annealing furnace for low temperature annealing. The annealing temperature was 200°C and the annealing time was 1.5 h.

[0045] Hereinafter, the inventors evaluated the wear resistance and fatigue life of the coatings in Examples 1-5 and Comparative Examples 1-2. Since the inner wall coating of the shaped hose is not convenient for testing, the inventors selected thin sheet of stainless steel as an alternative substrate, and used the coating preparation processes in Examples 1-5 and Comparative Examples 1-2 as alternative samples to evaluate the relevant properties of each group of coating sample samples, wherein the specific test method is as follows:

[0046] Wear resistance: The wear resistance of each sample coating was evaluated using a CETR-3 friction and wear tester with a load of 5N, a GCr15 steel ball with a diameter of 5mm, a friction frequency of 8Hz, a friction stroke of 3mm, and a friction time of 60min. An electronic balance was used to weigh the mass before and after wear to calculate the wear amount.

[0047] Fatigue life: Apply an alternating force of 500N to each test sample and record the number of times the force is applied until cracks appear in the coating material.

[0048] The specific experimental data are shown in Table 1.

[0049] Table 1

[0050] serial number Wear amount / mg Number of force / times Example 1 3.72 1361 Example 2 4.61 1174 Example 3 4.80 ＞1500 Example 4 5.32 ＞1500 Example 5 6.01 1199 Comparative Example 1 3.16 729 Comparative Example 2 12.39 ＞1500

[0051] As can be seen from Table 1, the MoS2 soft coating can effectively improve the wear resistance of the material, but it has the defect of insufficient fatigue strength. By adding Nb to the MoS2 soft coating, its fatigue life can be effectively improved. However, adding Nb will cause the wear resistance of the MoS2 soft coating to decrease. Therefore, the mass content of Nb in the coating needs to be controlled at 9wt%-22wt%.

[0052] In addition, the shaping hose for choledochoscope of the present invention can also be made of organic composite materials, and the coating treatment of the inner wall of the organic composite material can refer to the relevant method in the embodiment. It should be noted that the selected organic composite material must be able to withstand annealing treatment at 200°C.

[0053] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the technical principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing an inner wall coating of a shaped hose for a choledochoscope, It is characterized in that The preparation method comprises the following steps: The shaping hose for choledochoscope made of metal or organic composite material is placed in a mixed solution of acetic acid and HCl for polishing; the polished shaping hose is placed in a mixed solution of sodium carbonate and OP-10 emulsifier for degreasing; the degreasing shaping hose is ultrasonically cleaned with deionized water until there is no residual agent on the inner wall, and finally dried; Place the shaped hose into the sputtering coating machine and use a cylindrical target to coat the inner wall of the shaped hose with MoS 2 -Nb soft wear-resistant coating, in which the target material is MoS 2 -Nb composite target, the mass content of Nb in the target is 9wt%-22wt%, the sputtering process uses argon as the working gas, the sputtering pressure is 8Pa, the sputtering temperature is 120℃, the argon flow rate is 80sccm, and the sputtering time is 45min; The MoS 2 The shaped hose with -Nb soft coating is placed in a vacuum annealing furnace for low temperature annealing, the annealing temperature is 180-200°C, and the annealing time is 1.5-2.0h.

2. A preparation method as claimed in claim 1, It is characterized in that The concentration of the acetic acid is 20%.

3. A preparation method as claimed in claim 1, It is characterized in that The concentration of HCl is 10%.

4. A preparation method as claimed in claim 1, It is characterized in that The concentration of the sodium carbonate is 22%.

5. A preparation method as claimed in claim 1, It is characterized in that The concentration of the OP-10 emulsifier is 8%.

6. A preparation method as claimed in claim 1, It is characterized in that The drying process is performed under a nitrogen atmosphere.

7. An inner wall coating of a shaped hose for a choledochoscope, It is characterized in that The coating is prepared by the method according to any one of claims 1 to 6.