Traditional Chinese medicine acupuncture needle with nano graphene coating

Abstract

The invention belongs to the technical field of traditional Chinese medicine acupuncture needles, and particularly relates to a nano graphene coating traditional Chinese medicine acupuncture needle which comprises a traditional Chinese medicine acupuncture needle body, a nano graphene layer covers the portion from the needle point of the traditional Chinese medicine acupuncture needle body to the middle of the traditional Chinese medicine acupuncture needle body, and the nano graphene layer is made of medical-grade stainless steel or titanium alloy. A nano transition layer is arranged between the traditional Chinese medicine acupuncture needle body and the nano graphene layer, and the nano transition layer is made of medical-grade nano titanium, nano chromium or nano titanium nitride. The acupuncture needle has the advantages that the overall hardness and surface wear resistance of the acupuncture needle are improved, the sharpness of the needle tip is effectively maintained, the needle tip is prevented from being passivated too fast in the repeated puncture and disinfection process, the service life of the single acupuncture needle is prolonged, and the medical cost caused by the fact that the acupuncture needle is scrapped in advance is reduced.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine acupuncture needle technology, specifically a traditional Chinese medicine acupuncture needle with a nano-graphene coating. Background Technology

[0002] Acupuncture is one of the core methods of traditional Chinese medicine. It achieves therapeutic effects by inserting acupuncture needles into specific acupoints on the body, stimulating the flow of qi and blood through the meridians. Currently, most clinically used acupuncture needles are made of medical-grade stainless steel (such as 304 and 316L) or titanium alloy. While these materials possess basic biocompatibility, long-term clinical application has revealed numerous technical shortcomings. Specific problems and examples are as follows:

[0003] 1. Insufficient hardness and wear resistance, needle tip is prone to failure.

[0004] Traditional medical stainless steel acupuncture needles typically have a Vickers hardness of only HV500-HV800, making the needle tips prone to wear during repeated punctures of the skin and subcutaneous tissue, as well as during disinfection. For example, in a traditional Chinese medicine clinic treating patients with chronic lower back pain three times a week using traditional stainless steel acupuncture needles, after four treatments, the needle tips showed significant dulling (microscopic observation showed the needle tip radius increasing from an initial 0.1mm to 0.3mm). The patient's pain score during needle insertion increased from an initial 2 (VAS score) to 5. Doctors needed to increase the insertion force to achieve the desired depth, and some acupuncture needles had to be discarded prematurely due to severe wear. The average lifespan of a single needle was only 8-10 treatments, increasing medical costs.

[0005] 2. High surface friction coefficient, causing significant pain to patients.

[0006] Even after polishing, the surface roughness of traditional acupuncture needles remains relatively high (Ra approximately 0.5-1.0 μm), with a coefficient of friction typically greater than 0.3. In clinical practice, when performing foot acupuncture on patients with diabetic peripheral neuropathy, the thicker stratum corneum of the skin increases the frictional resistance between the acupuncture needle and the skin and subcutaneous tissue, easily triggering a pain stress response in patients. Statistics from a community health service center show that approximately 35% of patients refuse continuous treatment due to pain upon needle insertion when using traditional acupuncture needles, affecting treatment adherence.

[0007] 3. Insufficient biocompatibility, posing risks of infection and allergies.

[0008] Some traditional acupuncture needles undergo electroplating (such as chromium or nickel plating) to improve their appearance or corrosion resistance. However, the electroplated layer is prone to peeling off during repeated disinfection or puncture. For example, a hospital once reported a patient who experienced an allergic reaction due to the peeling of the chromium plating on an acupuncture needle, which came into contact with subcutaneous tissue, causing local redness, swelling, and oozing. Blood tests showed an eosinophil count of 8% (normal range 0.4%-8%). Although the patient recovered after a week of local anti-infection treatment, they subsequently refused acupuncture treatment. Furthermore, the surface of traditional acupuncture needles easily absorbs sweat and tissue fluid, and if disinfection is not thorough, bacteria can easily grow. A primary healthcare institution once reported two patients developing folliculitis at the puncture site (bacterial culture revealed Staphylococcus aureus) due to improper storage of traditional acupuncture needles.

[0009] 4. Poor corrosion resistance, making it difficult to adapt to various types of disinfection.

[0010] In clinical practice, acupuncture needles need to be sterilized using multiple methods, including 75% ethanol, chlorine-containing disinfectants (such as 500mg / L 84 disinfectant), and high-temperature and high-pressure sterilization (121℃, 0.1MPa). After traditional stainless steel acupuncture needles are immersed in chlorine-containing disinfectant 20 times (30 minutes each time), pitted corrosion (corrosion rate of about 5%) will appear on the surface. After high-temperature and high-pressure sterilization, the oxide layer on the surface will thicken, further reducing the surface smoothness. Although titanium alloy acupuncture needles have slightly better corrosion resistance, they are more expensive, and micro-cracks still exist on the surface after long-term sterilization, making it difficult to meet the high-frequency sterilization needs of primary healthcare institutions.

[0011] 5. Poor thermal conductivity, resulting in poor comfort.

[0012] Traditional acupuncture needles have low thermal conductivity (stainless steel approximately 15-20 W / (m·K), titanium alloy approximately 17 W / (m·K)), resulting in a significant temperature difference with human body temperature (37℃). In winter clinical treatment, the contact between the acupuncture needles and the skin can easily cause discomfort due to cold stimulation. Approximately 20% of sensitive patients (such as children and the elderly) require the doctor to preheat the needle tip by rubbing it with their hand, adding to the procedure. Furthermore, if combined with moxibustion ("warm needle moxibustion"), the uneven heat conduction of traditional acupuncture needles can easily lead to a temperature difference exceeding 5℃ between the needle tip and the needle tail, affecting the effectiveness of the warming therapy. 6. Lack of antibacterial properties; easily contaminated during long-term storage.

[0013] Traditional acupuncture needles lack active antibacterial function. In high-humidity storage environments (such as the rainy season in southern China, with relative humidity > 80%), even after disinfection, bacterial growth may still be observed in samples after 7 days of storage. A test conducted by a traditional Chinese medicine clinic showed that after 7 days of storage, the number of E. coli colonies in traditional acupuncture needles could reach 12-15 CFU / piece (far exceeding the requirement of ≤ 2 CFU / piece in the medical device hygiene standard). They need to be disinfected again before use, increasing the workload of medical staff.

[0014] In summary, existing acupuncture needles have shortcomings in terms of hardness, wear resistance, surface properties, biocompatibility, corrosion resistance, thermal conductivity, and antibacterial properties. Therefore, a nano-graphene coated acupuncture needle for traditional Chinese medicine has been invented. Summary of the Invention

[0015] To solve the above-mentioned technical problems, the present invention provides the following technical solution:

[0016] A traditional Chinese medicine acupuncture needle with a nano-graphene coating includes a traditional Chinese medicine acupuncture needle body, wherein the tip of the traditional Chinese medicine acupuncture needle body to the middle part of the traditional Chinese medicine acupuncture needle body is covered with a nano-graphene layer, and the material of the nano-graphene layer is medical-grade stainless steel or titanium alloy.

[0017] As a preferred embodiment of the traditional Chinese medicine acupuncture needle with nano-graphene coating described in this invention, a nano-transition layer is provided between the acupuncture needle body and the nano-graphene layer, and the material of the nano-transition layer is medical-grade nano-titanium, nano-chromium, or nano-titanium nitride.

[0018] As a preferred embodiment of the nano-graphene coated acupuncture needle of the present invention, it further includes a preparation method, the specific preparation steps of which are as follows:

[0019] S1, Substrate pretreatment:

[0020] S11, Degreasing: The body of the acupuncture needle is placed in an acetone solution for ultrasonic cleaning to remove surface oil.

[0021] S12, pickling: Immerse the degreased acupuncture needle body in a 5%-10% hydrochloric acid solution to remove the surface oxide layer;

[0022] S13, Polishing: Polishing is performed using an electrolytic polishing process to achieve a substrate surface roughness Ra≤0.05μm;

[0023] S14, Cleaning and Drying: Rinse the substrate three times with deionized water for two minutes each time, and then dry it in a vacuum drying oven;

[0024] S2, Substrate activation treatment:

[0025] S21, the pre-treated acupuncture needle body is fixed in the plasma processor cavity;

[0026] S22, first use a vacuum pump to evacuate to the target vacuum level, then introduce argon gas and adjust the flow rate to 12 sccm to maintain stable chamber pressure;

[0027] S23, turn on the RF power supply, and gradually increase it from 20W to 80-100W for processing;

[0028] S24, turn off the power and argon gas, continue to evacuate for 5-6 minutes, then fill with nitrogen gas to normal pressure, open the cavity, and take out the acupuncture needle body;

[0029] S3, Preparation of the nano-transition layer:

[0030] S31: Fix the activated TCM acupuncture needle body onto the sputtering instrument sample holder and close the cavity;

[0031] S32: First, use a vacuum pump to evacuate to the target vacuum level, then introduce argon gas and adjust the flow rate to 18 sccm to maintain the chamber pressure at 0.8 Pa;

[0032] S33: First, turn on the target cooling system, then turn on the RF power supply to 110W for pre-sputtering;

[0033] S34: After the temperature is raised to 160℃ and stabilized, timed deposition begins;

[0034] S35: After deposition is complete, turn off the power and argon gas, continue to evacuate for 5 minutes, then purge with nitrogen to atmospheric pressure and remove the acupuncture needle body;

[0035] S4, Graphene coating preparation:

[0036] S41, fix the body of the traditional Chinese medicine acupuncture needle with the nano-transition layer onto the HWCVD sample stage and close the reaction chamber;

[0037] S42, first use a vacuum pump to evacuate to the target vacuum level, then introduce hydrogen gas and adjust the flow rate to 18 sccm to maintain the deposition pressure of 18 Pa;

[0038] S43: Gradually increase the temperature to 1850-1900℃ and keep it warm;

[0039] S44: First, heat the temperature to 780-800℃ and stabilize it. Then, introduce methane and adjust the flow rate to 9 sccm. After adjusting CH4:H2 = 1:10, start timing and deposition for 30-32 minutes.

[0040] S45: After deposition is complete, first turn off the methane, continue to purge with hydrogen for 10 minutes, then turn off the heating and hydrogen.

[0041] S46: After the reaction chamber cools naturally, fill it with nitrogen to atmospheric pressure and remove the acupuncture needle body;

[0042] S5, Coating Defect Repair:

[0043] S51, fix the acupuncture needle body with the nano-graphene layer to the ALD sample holder and place it into the reaction chamber;

[0044] S52, first use a vacuum pump to evacuate to the target vacuum level, then heat to 130-140℃ and stabilize for 30-35 minutes;

[0045] S53: Set deposition cycle parameters: TMA pulse 0.15 seconds → purge 12 seconds → water pulse 0.08 seconds → purge 10 seconds, which is one cycle;

[0046] S54: Start the deposition process and complete 4 cycles;

[0047] S55: After deposition is complete, continue to evacuate for 10 minutes, purge with nitrogen to atmospheric pressure, and remove the acupuncture needle body;

[0048] S6, Post-processing:

[0049] S61: The body of the traditional Chinese medicine acupuncture needle is placed in a nitrogen atmosphere for annealing.

[0050] S62: After natural cooling to room temperature, a traditional Chinese medicine acupuncture needle with a nano-graphene coating is obtained.

[0051] As a preferred embodiment of the nano-graphene coated acupuncture needle of the present invention, wherein: the ultrasonic cleaning time in S11 is set to 15-20 minutes and the ultrasonic cleaning power is set to 300W; and the soaking time in S12 is set to 3-5 minutes.

[0052] As a preferred embodiment of the nano-graphene coated acupuncture needle of the present invention, wherein: the electrolyte in the electrolytic polishing process in S13 is a phosphoric acid-sulfuric acid mixture, and the volume ratio of phosphoric acid to sulfuric acid is 3:1; the polishing time in S13 is set to 5-8 minutes; the temperature of the vacuum drying oven in S14 is set to 80-100℃, and the drying time is set to 30-35 minutes.

[0053] As a preferred embodiment of the nano-graphene coated acupuncture needle of the present invention, wherein: the vacuum degree in S22 is set to 5x10 -2 Pa; The processing time in S23 is set to 4-6 minutes.

[0054] As a preferred embodiment of the nano-graphene coated acupuncture needle of the present invention, wherein: the vacuum degree in step S32 is set to 5 x 10⁻⁶. -4 Pa; the pre-sputtering time in S33 is set to 3-5 minutes.

[0055] As a preferred embodiment of the nano-graphene coated acupuncture needle of the present invention, wherein: the vacuum degree in step S42 is set to 5 x 10⁻⁶. -3 Pa; the heat preservation time in S43 is set to 10-12 minutes.

[0056] As a preferred embodiment of the nano-graphene coated acupuncture needle of the present invention, wherein the cooling temperature in S46 is set to below 200-220℃.

[0057] As a preferred embodiment of the nano-graphene coated acupuncture needle of the present invention, wherein: the vacuum degree in step S52 is set to 5 x 10⁻⁶. -3 Pa; the annealing temperature in S61 is set to 450-550℃, and the holding time is set to 20-30 minutes.

[0058] Compared with existing technologies:

[0059] 1. This invention improves the overall hardness and surface wear resistance of acupuncture needles, effectively maintains the sharpness of the needle tip, avoids the needle tip becoming dull too quickly during repeated punctures and disinfection, extends the service life of a single acupuncture needle, and reduces medical costs caused by premature scrapping of acupuncture needles.

[0060] 2. This invention reduces the surface friction coefficient of acupuncture needles, reduces frictional resistance with the skin and subcutaneous tissue during needle insertion, alleviates pain during needle insertion, reduces the likelihood of patients refusing continuous treatment due to pain, and improves treatment compliance.

[0061] 3. This invention improves the biocompatibility of acupuncture needles, avoiding allergic reactions caused by coating peeling (such as traditional electroplating) or contact between the substrate itself and human tissue; at the same time, it reduces the adsorption of sweat and tissue fluid on the substrate surface, reduces the risk of bacterial growth due to incomplete disinfection, and reduces the problem of infection at the puncture site.

[0062] 4. This invention enhances the corrosion resistance of acupuncture needles, enabling them to withstand various disinfection methods commonly used in clinical practice, such as ethanol, chlorine-containing disinfectants, and high-temperature and high-pressure disinfection. It avoids rust, thickening of the oxide layer, or micro-cracks on the surface after disinfection, thus meeting the high-frequency disinfection needs of primary healthcare institutions.

[0063] 5. This invention improves the thermal conductivity of acupuncture needles, enhances the uniformity of thermal conductivity, reduces the temperature difference between acupuncture needles and the human body, avoids the discomfort of cold stimulation during treatment in winter, and reduces the number of preheating steps for doctors; at the same time, it optimizes the temperature consistency between the needle tip and the needle tail in warm acupuncture therapy, improves the effect of warm therapy, and improves the overall treatment experience.

[0064] 6. This invention provides acupuncture needles with a long-term stable antibacterial function. Even in a high-humidity storage environment, it can reduce bacterial growth during the storage process after disinfection, eliminating the need for frequent re-disinfection, reducing the workload of medical staff, and ensuring the safety of acupuncture needles during storage. Attached Figure Description

[0065] Figure 1 This is a three-dimensional structural diagram of the present invention;

[0066] Figure 2 This is a cross-sectional view of the structure of the present invention;

[0067] Figure 3 This is a schematic diagram of the structure of the acupuncture needle of the present invention.

[0068] The image shows: the acupuncture needle body 10, the nano-transition layer 20, and the nano-graphene layer 30. Detailed Implementation

[0069] To make the objectives, technical solutions, and advantages of the present invention clearer, the embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.

[0070] Example 1:

[0071] This invention provides a traditional Chinese medicine acupuncture needle with a nano-graphene coating. Please refer to [link / reference]. Figures 1-3 The acupuncture needle body 10 is provided, and a nano-graphene layer 30 is provided from the tip of the acupuncture needle body 10 to the middle of the acupuncture needle body 10. The nano-graphene layer 30 is made of medical grade stainless steel (304 / 316L) or titanium alloy. The thickness of the nano-graphene layer 30 is 50nm, the carbon purity is ≥99.9%, the Vickers hardness is ≥HV2300, and the coefficient of friction is ≤0.1.

[0072] A nano-transition layer 20 is provided between the acupuncture needle body 10 and the nano-graphene layer 30. The material of the nano-transition layer 20 is medical-grade nano-titanium, nano-chromium, or nano-titanium nitride.

[0073] It also includes a preparation method, the specific preparation steps of which are as follows:

[0074] S1, Substrate pretreatment:

[0075] S11, Degreasing: The body of the acupuncture needle 10 is placed in an acetone solution for ultrasonic cleaning to remove surface oil; the ultrasonic cleaning time is set to 15 minutes and the ultrasonic cleaning power is set to 300W.

[0076] S12, pickling: Immerse the degreased acupuncture needle body 10 in a 5% hydrochloric acid solution to remove the surface oxide layer; the immersion time is set to 3 minutes.

[0077] S13, Polishing: Polishing is performed using an electrolytic polishing process to achieve a substrate surface roughness Ra≤0.05μm; wherein, the electrolyte in the electrolytic polishing process is a phosphoric acid-sulfuric acid mixture, and the volume ratio of phosphoric acid to sulfuric acid is 3:1; in addition, the polishing time is set to 5 minutes;

[0078] S14, Cleaning and Drying: Rinse the substrate three times with deionized water for 2 minutes each time, and then dry it in a vacuum drying oven; the temperature of the vacuum drying oven is set to 80℃ and the drying time is set to 30 minutes.

[0079] S2, Substrate activation treatment:

[0080] S21, the pre-treated acupuncture needle body 10 is fixed in the plasma processor cavity;

[0081] S22, first, the vacuum pump is used to evacuate to the target vacuum level, then argon gas is introduced and the flow rate is adjusted to 12 sccm to maintain stable chamber pressure; the vacuum level is set to 5 x 10 -2 Pa;

[0082] S23, turn on the RF power supply and gradually increase it from 20W to 80W for processing; the processing time is set to 4 minutes.

[0083] S24, turn off the power and argon gas, continue to evacuate for 5 minutes, then fill with nitrogen gas to normal pressure, open the cavity, and take out the TCM acupuncture needle body 10;

[0084] S3, Preparation of the nano-transition layer:

[0085] S31: Fix the activated TCM acupuncture needle body 10 to the sputtering instrument sample holder (the distance between the sample holder and the target material is 10cm), and close the cavity;

[0086] S32: First, evacuate to the target vacuum level using a vacuum pump, then introduce argon gas and adjust the flow rate to 18 sccm to maintain the chamber pressure at 0.8 Pa; the vacuum level is set to 5 x 10⁻⁶ Pa. -4 Pa;

[0087] S33: First, turn on the target cooling system (water temperature 25℃), then turn on the RF power supply to 110W for pre-sputtering; the pre-sputtering time is set to 3 minutes.

[0088] S34: After heating to 160℃ and stabilizing, start timed deposition (Ti target deposition for 12.5 minutes, thickness 10nm);

[0089] S35: After deposition is complete, turn off the power and argon gas, continue to evacuate for 5 minutes, then fill with nitrogen to normal pressure, and take out the acupuncture needle body 10;

[0090] S4, Graphene coating preparation:

[0091] S41, fix the TCM acupuncture needle body 10 with nano-transition layer 20 on the HWCVD sample stage (the distance between the sample stage and the hot wire is 8cm) and close the reaction chamber.

[0092] S42, first, the target vacuum level is achieved using a vacuum pump, then hydrogen gas is introduced and the flow rate is adjusted to 18 sccm, maintaining a deposition pressure of 18 Pa; wherein, the vacuum level is set to 5 x 10 -3 Pa;

[0093] S43: Gradually increase the temperature to 1850℃ and hold it at that temperature for 10 minutes.

[0094] S44: First, heat the temperature to 780℃ and stabilize it. Then, introduce methane and adjust the flow rate to 9 sccm. After adjusting CH4:H2 = 1:10, start timing and deposition for 30 minutes.

[0095] S45: After deposition is complete, first turn off the methane, continue to purge with hydrogen for 10 minutes, then turn off the heating and hydrogen.

[0096] S46: After the reaction chamber cools naturally, fill it with nitrogen to atmospheric pressure and remove the acupuncture needle body 10; the cooling temperature is set to below 200℃.

[0097] S5, Coating Defect Repair:

[0098] S51, fix the acupuncture needle body 10 with the nano-graphene layer 30 to the ALD sample holder (the sample holder temperature is controllable) and place it into the reaction chamber.

[0099] S52, firstly, the vacuum pump is used to evacuate to the target vacuum level, then the temperature is raised to 130℃ and stabilized for 30 minutes; the vacuum level is set to 5 x 10. -3 Pa;

[0100] S53: Set deposition cycle parameters: TMA pulse 0.15 seconds → purge 12 seconds → water pulse 0.08 seconds → purge 10 seconds, which is one cycle;

[0101] S54: Start the deposition process and complete 4 cycles;

[0102] S55: After deposition is complete, continue to evacuate for 10 minutes, fill with nitrogen to normal pressure, and take out the acupuncture needle body 10;

[0103] S6, Post-processing:

[0104] S61: Place the acupuncture needle body 10 in a nitrogen atmosphere and perform annealing treatment; wherein the annealing temperature is set to 450℃ and the holding time is set to 20 minutes.

[0105] S62: After natural cooling to room temperature, a traditional Chinese medicine acupuncture needle with a nano-graphene coating is obtained.

[0106] Example 2:

[0107] This invention provides a traditional Chinese medicine acupuncture needle with a nano-graphene coating. Please refer to [link / reference]. Figures 1-3 The acupuncture needle body 10 is provided, and a nano-graphene layer 30 is provided from the tip of the acupuncture needle body 10 to the middle of the acupuncture needle body 10. The nano-graphene layer 30 is made of medical grade stainless steel (304 / 316L) or titanium alloy. The thickness of the nano-graphene layer 30 is 125nm, the carbon purity is ≥99.9%, the Vickers hardness is ≥HV2300, and the coefficient of friction is ≤0.1.

[0108] A nano-transition layer 20 is provided between the acupuncture needle body 10 and the nano-graphene layer 30. The material of the nano-transition layer 20 is medical-grade nano-titanium, nano-chromium, or nano-titanium nitride.

[0109] It also includes a preparation method, the specific preparation steps of which are as follows:

[0110] S1, Substrate pretreatment:

[0111] S11, Degreasing: The body of the acupuncture needle 10 is placed in an acetone solution for ultrasonic cleaning to remove surface oil; the ultrasonic cleaning time is set to 17.5 minutes and the ultrasonic cleaning power is set to 300W.

[0112] S12, pickling: Immerse the degreased acupuncture needle body 10 in a 7.5% hydrochloric acid solution to remove the surface oxide layer; the immersion time is set to 4 minutes.

[0113] S13, Polishing: Polishing is performed using an electrolytic polishing process to achieve a substrate surface roughness Ra≤0.05μm; wherein the electrolyte for the electrolytic polishing process is a phosphoric acid-sulfuric acid mixture, and the volume ratio of phosphoric acid to sulfuric acid is 3:1; in addition, the polishing time is set to 6.5 minutes;

[0114] S14, Cleaning and Drying: Rinse the substrate three times with deionized water for two minutes each time, and then dry it in a vacuum drying oven; the temperature of the vacuum drying oven is set to 90℃ and the drying time is set to 32.5 minutes.

[0115] S2, Substrate activation treatment:

[0116] S21, the pre-treated acupuncture needle body 10 is fixed in the plasma processor cavity;

[0117] S22, first, the vacuum pump is used to evacuate to the target vacuum level, then argon gas is introduced and the flow rate is adjusted to 12 sccm to maintain stable chamber pressure; the vacuum level is set to 5 x 10 -2 Pa;

[0118] S23, turn on the RF power supply, and gradually increase it from 20W to 90W for processing; the processing time is set to 5 minutes.

[0119] S24, turn off the power and argon gas, continue to evacuate for 5.5 minutes, then fill with nitrogen gas to normal pressure, open the cavity, and take out the TCM acupuncture needle body 10;

[0120] S3, Preparation of the nano-transition layer:

[0121] S31: Fix the activated TCM acupuncture needle body 10 to the sputtering instrument sample holder (the distance between the sample holder and the target material is 10cm), and close the cavity;

[0122] S32: First, evacuate to the target vacuum level using a vacuum pump, then introduce argon gas and adjust the flow rate to 18 sccm to maintain the chamber pressure at 0.8 Pa; the vacuum level is set to 5 x 10⁻⁶ Pa. -4 Pa;

[0123] S33: First, turn on the target cooling system (water temperature 25℃), then turn on the RF power supply to 110W for pre-sputtering; the pre-sputtering time is set to 4 minutes.

[0124] S34: After heating to 160℃ and stabilizing, start timed deposition (Ti target deposition for 12.5 minutes, thickness 10nm);

[0125] S35: After deposition is complete, turn off the power and argon gas, continue to evacuate for 5 minutes, then fill with nitrogen to normal pressure, and take out the acupuncture needle body 10;

[0126] S4, Graphene coating preparation:

[0127] S41, fix the TCM acupuncture needle body 10 with nano-transition layer 20 on the HWCVD sample stage (the distance between the sample stage and the hot wire is 8cm) and close the reaction chamber.

[0128] S42, first, the target vacuum level is achieved using a vacuum pump, then hydrogen gas is introduced and the flow rate is adjusted to 18 sccm, maintaining a deposition pressure of 18 Pa; wherein, the vacuum level is set to 5 x 10 -3 Pa;

[0129] S43: Gradually increase the temperature to 1875℃ and hold it at that temperature; the holding time is set to 11 minutes.

[0130] S44: First, heat the temperature to 790℃ and stabilize it. Then, introduce methane and adjust the flow rate to 9 sccm. After adjusting CH4:H2 = 1:10, start timing and deposition for 31 minutes.

[0131] S45: After deposition is complete, first turn off the methane, continue to purge with hydrogen for 10 minutes, then turn off the heating and hydrogen.

[0132] S46: After the reaction chamber cools naturally, fill it with nitrogen to atmospheric pressure and remove the acupuncture needle body 10; the cooling temperature is set to below 210℃.

[0133] S5, Coating Defect Repair:

[0134] S51, fix the acupuncture needle body 10 with the nano-graphene layer 30 to the ALD sample holder (the sample holder temperature is controllable) and place it into the reaction chamber.

[0135] S52, firstly, the vacuum pump is used to evacuate to the target vacuum level, then the temperature is raised to 135℃ and stabilized for 32.5 minutes; the vacuum level is set to 5 x 10. -3 Pa;

[0136] S53: Set deposition cycle parameters: TMA pulse 0.15 seconds → purge 12 seconds → water pulse 0.08 seconds → purge 10 seconds, which is one cycle;

[0137] S54: Start the deposition process and complete 4 cycles;

[0138] S55: After deposition is complete, continue to evacuate for 10 minutes, fill with nitrogen to normal pressure, and take out the acupuncture needle body 10;

[0139] S6, Post-processing:

[0140] S61: Place the acupuncture needle body 10 in a nitrogen atmosphere and perform annealing treatment; wherein the annealing temperature is set to 500℃ and the holding time is set to 25 minutes.

[0141] S62: After natural cooling to room temperature, a traditional Chinese medicine acupuncture needle with a nano-graphene coating is obtained.

[0142] Example 3:

[0143] This invention provides a traditional Chinese medicine acupuncture needle with a nano-graphene coating. Please refer to [link / reference]. Figures 1-3 The acupuncture needle body 10 is provided, and a nano-graphene layer 30 is provided from the tip of the acupuncture needle body 10 to the middle of the acupuncture needle body 10. The nano-graphene layer 30 is made of medical grade stainless steel (304 / 316L) or titanium alloy. The thickness of the nano-graphene layer 30 is 200nm, the carbon purity is ≥99.9%, the Vickers hardness is ≥HV2300, and the coefficient of friction is ≤0.1.

[0144] A nano-transition layer 20 is provided between the acupuncture needle body 10 and the nano-graphene layer 30. The material of the nano-transition layer 20 is medical-grade nano-titanium, nano-chromium, or nano-titanium nitride.

[0145] It also includes a preparation method, the specific preparation steps of which are as follows:

[0146] S1, Substrate pretreatment:

[0147] S11, Degreasing: The body of the acupuncture needle 10 is placed in an acetone solution for ultrasonic cleaning to remove surface oil; the ultrasonic cleaning time is set to 20 minutes and the ultrasonic cleaning power is set to 300W.

[0148] S12, pickling: Immerse the degreased acupuncture needle body 10 in a 10% hydrochloric acid solution to remove the surface oxide layer; the immersion time is set to 5 minutes.

[0149] S13, Polishing: Polishing is performed using an electrolytic polishing process to achieve a substrate surface roughness Ra≤0.05μm; wherein, the electrolyte in the electrolytic polishing process is a phosphoric acid-sulfuric acid mixture, and the volume ratio of phosphoric acid to sulfuric acid is 3:1; in addition, the polishing time is set to 8 minutes;

[0150] S14, Cleaning and Drying: Rinse the substrate three times with deionized water for 2 minutes each time, and then dry it in a vacuum drying oven; the temperature of the vacuum drying oven is set to 100℃ and the drying time is set to 35 minutes.

[0151] S2, Substrate activation treatment:

[0152] S21, the pre-treated acupuncture needle body 10 is fixed in the plasma processor cavity;

[0153] S22, first, the vacuum pump is used to evacuate to the target vacuum level, then argon gas is introduced and the flow rate is adjusted to 12 sccm to maintain stable chamber pressure; the vacuum level is set to 5 x 10 -2 Pa;

[0154] S23, turn on the RF power supply and gradually increase it from 20W to 100W for processing; the processing time is set to 6 minutes.

[0155] S24, turn off the power and argon gas, continue to evacuate for 6 minutes, then fill with nitrogen gas to normal pressure, open the cavity, and take out the TCM acupuncture needle body 10;

[0156] S3, Preparation of the nano-transition layer:

[0157] S31: Fix the activated TCM acupuncture needle body 10 to the sputtering instrument sample holder (the distance between the sample holder and the target material is 10cm), and close the cavity;

[0158] S32: First, evacuate to the target vacuum level using a vacuum pump, then introduce argon gas and adjust the flow rate to 18 sccm to maintain the chamber pressure at 0.8 Pa; the vacuum level is set to 5 x 10⁻⁶ Pa. -4 Pa;

[0159] S33: First, turn on the target cooling system (water temperature 25℃), then turn on the RF power supply to 110W for pre-sputtering; the pre-sputtering time is set to 5 minutes.

[0160] S34: After heating to 160℃ and stabilizing, start timed deposition (Ti target deposition for 12.5 minutes, thickness 10nm);

[0161] S35: After deposition is complete, turn off the power and argon gas, continue to evacuate for 5 minutes, then fill with nitrogen to normal pressure, and take out the acupuncture needle body 10;

[0162] S4, Graphene coating preparation:

[0163] S41, fix the TCM acupuncture needle body 10 with nano-transition layer 20 on the HWCVD sample stage (the distance between the sample stage and the hot wire is 8cm) and close the reaction chamber.

[0164] S42, first, the target vacuum level is achieved using a vacuum pump, then hydrogen gas is introduced and the flow rate is adjusted to 18 sccm, maintaining a deposition pressure of 18 Pa; wherein, the vacuum level is set to 5 x 10 -3 Pa;

[0165] S43: Gradually increase the temperature to 1900℃ and hold it at that temperature for 12 minutes.

[0166] S44: First, heat the temperature to 800℃ and stabilize it. Then, introduce methane and adjust the flow rate to 9 sccm. After adjusting CH4:H2 = 1:10, start timing and deposition for 32 minutes.

[0167] S45: After deposition is complete, first turn off the methane, continue to purge with hydrogen for 10 minutes, then turn off the heating and hydrogen.

[0168] S46: After the reaction chamber cools naturally, fill it with nitrogen to atmospheric pressure and remove the acupuncture needle body 10; the cooling temperature is set to below 220℃.

[0169] S5, Coating Defect Repair:

[0170] S51, fix the acupuncture needle body 10 with the nano-graphene layer 30 to the ALD sample holder (the sample holder temperature is controllable) and place it into the reaction chamber.

[0171] S52, firstly, the vacuum pump is used to evacuate to the target vacuum level, then the temperature is raised to 140℃ and stabilized for 35 minutes; the vacuum level is set to 5 x 10. -3 Pa;

[0172] S53: Set deposition cycle parameters: TMA pulse 0.15 seconds → purge 12 seconds → water pulse 0.08 seconds → purge 10 seconds, which is one cycle;

[0173] S54: Start the deposition process and complete 4 cycles;

[0174] S55: After deposition is complete, continue to evacuate for 10 minutes, fill with nitrogen to normal pressure, and take out the acupuncture needle body 10;

[0175] S6, Post-processing:

[0176] S61: Place the acupuncture needle body 10 in a nitrogen atmosphere and perform annealing treatment; wherein the annealing temperature is set to 550℃ and the holding time is set to 30 minutes.

[0177] S62: After natural cooling to room temperature, a traditional Chinese medicine acupuncture needle with a nano-graphene coating is obtained.

[0178] The following data were obtained by comparing the nano-graphene-coated acupuncture needles prepared in Examples 1-3 above:

[0179]

[0180] As shown in the table above, the nano-graphene coated acupuncture needles prepared in Examples 1-3 all exhibit good performance in terms of hardness and wear resistance. After use, Example 2 showed the best results.

[0181] Although the present invention has been described above with reference to embodiments, various modifications can be made and components can be replaced with equivalents without departing from the scope of the invention. In particular, as long as there is no structural conflict, the features in the disclosed embodiments can be combined with each other in any manner. The lack of an exhaustive description of these combinations in this specification is merely for the sake of brevity and resource conservation. Therefore, the present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

Claims

1. A nanographene-coated traditional Chinese medicine acupuncture needle comprising a traditional Chinese medicine acupuncture needle body (10), characterized in that, The tip of the traditional Chinese acupuncture needle body (10) to the middle of the traditional Chinese acupuncture needle body (10) is covered with a nano graphene layer (30), and the material of the nano graphene layer (30) is medical-grade stainless steel or titanium alloy.

2. A nanographene coated traditional Chinese medicine acupuncture needle according to claim 1, characterized in that, A nano transition layer (20) is arranged between the traditional Chinese acupuncture needle body (10) and the nano graphene layer (30), and the material of the nano transition layer (20) is medical-grade nano titanium, nano chromium or nano titanium nitride.

3. A nanographene coated traditional Chinese medicine acupuncture needle according to claim 1, characterized in that, Also includes a preparation method, the preparation steps are as follows: S1, substrate pretreatment: S11, degreasing: the traditional Chinese acupuncture needle body (10) is placed in acetone solution for ultrasonic cleaning, and the surface oil is removed; S12, pickling: the traditional Chinese acupuncture needle body (10) after degreasing is soaked in 5%-10% hydrochloric acid solution, and the surface oxide layer is removed; S13, polishing: electrolytic polishing process is adopted for polishing, so that the surface roughness Ra of the substrate is less than or equal to 0.05μm; S14, cleaning and drying: the substrate is washed with deionized water for 3 times, each time for 2 minutes, and then dried in a vacuum drying oven; S2, substrate activation treatment: S21, the traditional Chinese acupuncture needle body (10) after pretreatment is fixed in the cavity of the plasma treatment instrument; S22, first vacuum pump to the target vacuum degree, then argon is introduced and the flow is adjusted to 12sccm, and the cavity pressure is maintained stable; S23, start the radio frequency power supply, gradually increase from 20W to 80-100W for processing; S24, turn off the power and argon, continue to vacuum for 5-6 minutes, then fill nitrogen to normal pressure, open the cavity, take out the traditional Chinese acupuncture needle body (10); S3, nano transition layer preparation: S31: the activated traditional Chinese acupuncture needle body (10) is fixed on the sample holder of the sputtering instrument, and the cavity is closed; S32: first vacuum pump to the target vacuum degree, then argon is introduced and the flow is adjusted to 18sccm, and the cavity pressure is maintained at 0.8Pa; S33: first start the target cooling system, then start the radio frequency power supply and increase to 110W for pre-sputtering; S34: after heating to 160℃ and stabilizing, start timing deposition; S35: after deposition is completed, the power and argon are turned off, vacuum is continued for 5 minutes, then nitrogen is filled to normal pressure, and the traditional Chinese acupuncture needle body (10) is taken out; S4, graphene coating preparation: S41, the traditional Chinese acupuncture needle body (10) with nano transition layer (20) is fixed on the HWCVD sample table, and the reaction cavity is closed; S42, first vacuum pump to the target vacuum degree, then hydrogen is introduced and the flow is adjusted to 18sccm, and the deposition pressure is maintained at 18Pa; S43: gradually heat to 1850-1900℃, and keep warm; S44: first heat to 780-800℃ and stabilize, then introduce methane and adjust the flow to 9sccm, after adjusting CH4:H2=1:10, start timing deposition for 30-32 minutes; S45: after deposition is completed, first close the methane, continue to introduce hydrogen for 10 minutes, then close the heating and hydrogen; S46: after the reaction cavity is naturally cooled, nitrogen is filled to normal pressure, and the traditional Chinese acupuncture needle body (10) is taken out; S5, coating defect repair: S51, fix the TCM acupuncture needle body (10) with nano graphene layer (30) on the ALD sample holder and put it into the reaction cavity; S52, first, vacuumize to the target vacuum degree, then, heat to 130-140℃ and stabilize for 30-35 minutes; S53, set the deposition cycle parameters: TMA pulse 0.15 seconds→purge 12 seconds→water pulse 0.08 seconds→purge 10 seconds, 1 cycle; S54, start the deposition program, complete 4 cycles; S55, after the deposition, continue vacuumizing for 10 minutes, fill nitrogen to normal pressure, and take out the TCM acupuncture needle body (10); S6, post-processing: S61, place the TCM acupuncture needle body (10) in the nitrogen atmosphere and perform annealing treatment; S62, then, naturally cool to room temperature to obtain the nano graphene coated TCM acupuncture needle.

4. A nanographene coated traditional Chinese medicine acupuncture needle according to claim 3, characterized in that, In the S11, the ultrasonic cleaning time is set to 15-20 minutes and the ultrasonic cleaning power is set to 300W; in the S12, the soaking time is set to 3-5 minutes.

5. A nanographene coated traditional Chinese medicine acupuncture needle according to claim 3, characterized in that, In the S13, the electrolyte of the electrolytic polishing process is a phosphoric acid-sulfuric acid mixed solution, and the volume ratio of phosphoric acid to sulfuric acid is 3:1; the polishing time in the S13 is set to 5-8 minutes; the temperature of the vacuum drying oven in the S14 is set to 80-100℃, and the drying time is set to 30-35 minutes.

6. A nanographene coated traditional Chinese medicine acupuncture needle according to claim 3, characterized in that, The vacuum degree in S22 is set to 5x10 -2 Pa; the processing time in S23 is set to 4-6 minutes.

7. A nanographene coated traditional Chinese medicine acupuncture needle according to claim 3, characterized in that, The vacuum degree in S32 is set to 5x10 -4 Pa; the pre-sputtering time in S33 is set to 3-5 minutes.

8. A nanographene coated traditional Chinese medicine acupuncture needle according to claim 3, characterized in that, The vacuum degree in S42 is set to 5x10 -3 Pa; the holding time in S43 is set to 10-12 minutes.

9. A nanographene coated traditional Chinese medicine acupuncture needle according to claim 3, characterized in that, In the S46, the cooling temperature is set to 200-220℃ or below.

10. The nanographene coated traditional Chinese medicine acupuncture needle according to claim 3, characterized in that, The vacuum degree in S52 is set to 5x10 -3 Pa; the temperature during the annealing treatment in S61 is set to 450-550℃, and the holding time is set to 20-30 minutes.

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