An ultrathin seamless thin-walled tube and a method for manufacturing the same

Abstract

The application discloses an ultrathin seamless thin-walled pipe and a preparation method thereof, and belongs to the technical field of ultrathin pipe preparation. The preparation method comprises the following steps: after pretreatment of a substrate, glue coating treatment is performed on the outer wall of the substrate, and then soft baking treatment is performed; a film is prepared on the outer wall of the substrate after the soft baking treatment by adopting a physical vapor deposition technology, so that a substrate with a deposited film is obtained; the substrate with the deposited film is subjected to ultraviolet exposure treatment and glue removal treatment in sequence, so that a separated film is obtained; after post-treatment of the separated film, an ultrathin seamless thin-walled pipe is obtained; the method overcomes the limitation of a traditional mechanical processing technology on the diameter-thickness ratio of the pipe and the problem that a thin-walled plate cannot be used for curling connection due to the excessively thin pipe wall, the process is simple, the energy consumption is low, the precision is high, and mass production of various ultrathin seamless thin-walled pipes can be realized. The obtained ultrathin seamless thin-walled pipe has nanometer-level wall thickness control precision and surface roughness, and has a wide application prospect.

Description

Technical Field

[0001] This invention belongs to the field of ultrathin tube preparation technology, specifically relating to an ultrathin seamless thin-walled tube and its preparation method. Background Technology

[0002] Ultrathin seamless wall tubes, as a type of special tubing with a diameter-to-wall-thickness ratio exceeding 100, have become an indispensable key material in high-end equipment in aerospace, biomedicine, and nuclear industries. They also represent a critical technological bottleneck that urgently needs to be addressed in the automation and industrial chain development of advanced equipment manufacturing. With the increasing demand for ultrathin seamless wall tubes of extreme dimensions across various fields, especially those with outer diameters ranging from 3 to 1000 mm and wall thicknesses from 0.015 to 0.030 mm, they have become a crucial basic material urgently needed in many cutting-edge technology fields.

[0003] Traditional manufacturing processes involve complex multi-step steps, including high-energy-consumption casting of billets, high-load hot forging, hot rolling piercing, multi-pass hot rolling thinning, high-energy-consumption heat treatment, cold rolling sizing, and straightening. The resulting ultrathin seamless tubes generally suffer from poor microstructure uniformity, uneven wall thickness, large deformation force, and susceptibility to cracking. They are also accompanied by high energy consumption, high cost, low yield, and difficulty in producing high-quality ultrathin seamless tubes. For example, Chinese patent application CN112371752A achieves micron-level ultrathin copper tubes with a maximum wall thickness of 0.08-0.15 mm through a segmented floating drawing process. Similarly, Chinese patent application CN117086122A produces ultrathin copper tubes for micro heat pipes with a wall thickness of 0.055-0.060 mm by repeatedly cold-deforming and annealing pre-formed tubular copper material. These preparation methods still inherit the complexity and high energy consumption of traditional processes, and it is difficult to achieve stable production of high-precision, high-quality ultra-thin seamless tubes.

[0004] Although the development of additive manufacturing technology has made it possible to simplify processes and reduce energy consumption, Chinese patent application CN117718494A uses 3D printing technology to prepare small-diameter thin-walled tube blanks and performs heat treatment, followed by rolling and drawing to produce small-diameter ultrathin tubes with outer diameters of 0.9~4.0 mm and wall thicknesses of 0.04~0.08 mm. However, this method still relies on traditional machining, resulting in limited precision control, and the material range is limited to easily machinable metals and alloys, which cannot meet the needs of preparing ultrathin seamless tubes for semiconductors and ceramics.

[0005] Therefore, it is evident that developing a method with simple process, low energy consumption, high precision, and the ability to mass-produce various ultra-thin seamless thin-walled tubes has significant engineering practical value and economic benefits. Summary of the Invention

[0006] The purpose of this invention is to provide an ultrathin seamless thin-walled tube and its preparation method, so as to solve the technical problem that existing preparation methods are difficult to mass-produce due to complex processes and high preparation requirements.

[0007] To achieve the above objectives, the present invention employs the following technical solution:

[0008] This invention discloses a method for preparing an ultrathin seamless thin-walled tube, comprising the following steps:

[0009] After pretreatment of the substrate, adhesive is applied to the outer wall of the substrate, followed by soft baking.

[0010] A thin film was prepared on the outer wall of a substrate after soft baking using physical vapor deposition technology, resulting in a substrate with deposited thin film.

[0011] The substrate with the deposited thin film is subjected to UV exposure and resist removal treatment in sequence to obtain the detached thin film;

[0012] After post-processing, the detached membrane is used to obtain an ultra-thin seamless thin-walled tube.

[0013] Further, the pretreatment step is as follows: the substrate is ultrasonically cleaned in acetone and anhydrous ethanol solution for 10-30 min in sequence, and then dried;

[0014] The substrate is a glass tube; the material of the glass tube is alumina, sapphire, or quartz glass.

[0015] Furthermore, the coating process involves uniformly coating the outer wall of the substrate with a positive photoresist; the positive photoresist is any one of diazoquinone, polyimide, methacrylic acid, epoxy resin, and acrylic resin.

[0016] The adhesive application method is dip coating, spray coating, brush coating, drop coating, roller coating, electrostatic coating, or ultrasonic coating; the thickness of the adhesive coating is 0.001~0.01 mm.

[0017] Furthermore, the softening process is carried out at a temperature of 90~100 ℃ for a time of 10~60 s.

[0018] Furthermore, the physical vapor deposition technique is any one of vacuum evaporation deposition, sputtering deposition, and ion plating;

[0019] The material used to prepare the thin film is one of metal, alloy, semiconductor or ceramic;

[0020] The materials used to prepare the thin film are multilayer or composite materials made of metals, alloys, semiconductors or ceramics in free combination.

[0021] Furthermore, the step of sequentially performing ultraviolet exposure treatment on the substrate with the deposited thin film involves performing ultraviolet exposure treatment on the inner wall of the glass tube with the deposited thin film; the ultraviolet light source used in the ultraviolet exposure treatment is one of g-line, i-line, KrF-line, and ArF-line;

[0022] The ultraviolet exposure treatment time is 15~50 s.

[0023] Furthermore, the adhesive removal process is performed using a wet adhesive removal method; the wet adhesive removal time is 5-30 minutes; the adhesive removal reagent used in the wet adhesive removal process is one or more of acetone, ethanol, isopropanol, sodium hydroxide, potassium hydroxide, 1-methyl-2-pyrrolidone, aziridine pyrrolidone, dimethyl sulfoxide, and tetramethylammonium hydroxide.

[0024] Furthermore, the outer diameter of the substrate is 1~100 mm.

[0025] The present invention also discloses an ultrathin seamless thin-walled tube prepared by the above preparation method.

[0026] Furthermore, the inner diameter of the ultrathin seamless thin-walled tube is 1~100 mm, and the wall thickness is 0.001~0.05 mm.

[0027] Compared with the prior art, the present invention has the following beneficial effects:

[0028] This invention discloses a method for preparing ultrathin seamless thin-walled tubes. Based on physical vapor deposition technology, a thin film is deposited on the substrate surface, which overcomes the limitations of traditional machining processes on the diameter-to-thickness ratio of the tube and the problem that thin-walled plates cannot be used for rolling and connecting due to the excessive thinness of the tube wall. The method is simple, energy-efficient, and highly accurate, and can realize the mass production of various ultrathin seamless thin-walled tubes. It has important engineering practical value and economic benefits.

[0029] Furthermore, the physical vapor deposition technology employed encompasses vacuum evaporation deposition, sputtering deposition, and ion plating. The constituent materials of the ultrathin seamless thin-walled tube include various metals, alloys, semiconductors, ceramics, and multilayer or composite materials freely combined from them. It has strong versatility, enabling high-precision, large-scale industrial production and facilitating widespread application.

[0030] The present invention also discloses an ultrathin seamless thin-walled tube prepared by the above preparation method. The wall thickness of the prepared ultrathin seamless thin-walled tube is 0.001~0.05 mm. Its wall structure and thickness are uniform, and it has nanoscale wall thickness control precision and surface roughness, which has broad application prospects. Attached Figure Description

[0031] Figure 1This is a process flow diagram of the method for preparing ultrathin seamless thin-walled tubes according to the present invention. Detailed Implementation

[0032] To enable those skilled in the art to understand the features and effects of the present invention, the terms and expressions used in the specification and claims are explained and defined in general below. Unless otherwise specified, all technical and scientific terms used herein have the ordinary meaning understood by those skilled in the art regarding the present invention, and in case of conflict, the definitions in this specification shall prevail.

[0033] The theories or mechanisms described and disclosed herein, whether right or wrong, should not in any way limit the scope of the invention, that is, the contents of the invention can be implemented without being limited by any particular theory or mechanism.

[0034] In this document, all features defined by numerical ranges or percentage ranges, such as numerical values, quantities, contents, and concentrations, are for the sake of brevity and convenience only. Accordingly, descriptions of numerical ranges or percentage ranges should be considered as covering and specifically disclosing all possible sub-ranges and individual numerical values ​​(including integers and fractions) within those ranges.

[0035] In this article, unless otherwise specified, “contains,” “includes,” “containing,” “has,” or similar terms cover the meanings of “composed of” and “mainly composed of,” for example, “A contains a” covers the meanings of “A contains a and others” and “A contains only a.”

[0036] For the sake of brevity, not all possible combinations of the technical features in each implementation scheme or embodiment are described herein. Therefore, as long as there is no contradiction in the combination of these technical features, the technical features in each implementation scheme or embodiment can be combined arbitrarily, and all possible combinations should be considered within the scope of this specification.

[0037] This invention provides a method for fabricating an ultrathin seamless thin-walled tube based on physical vapor deposition (PVD) technology. PVD technology encompasses vacuum evaporation, sputtering, and ion plating, including but not limited to resistance heating evaporation, electron beam evaporation, induction heating evaporation, magnetron sputtering, radio frequency sputtering, ion beam sputtering, magnetron sputtering ion plating, vacuum evaporation ion plating, and multi-arc ion plating. The ultrathin seamless thin-walled tube is composed of various metals, alloys, semiconductors, ceramics, and multilayer or composite materials freely combined from them. Figure 1 As shown, the main steps include:

[0038] S1, Pretreatment: Select a substrate with an outer diameter of 1~100 mm, ultrasonically clean it in acetone and anhydrous ethanol solution for 10~30 min in sequence, and then dry it.

[0039] S2, Coating: Use positive photoresist to uniformly coat the outer wall of the pretreated substrate;

[0040] S3, Soft baking: Place the substrate with uniformly coated photoresist on a hot plate or in an oven for soft baking treatment; the temperature is 90~100 ℃ and the time is 10~60 s;

[0041] S4, Physical Vapor Deposition: The substrate after soft baking is placed into the deposition chamber, and a thin film with a thickness of 0.001~0.05 mm is formed on its outer wall using physical vapor deposition technology;

[0042] S5, UV exposure: The inner wall of the substrate with the deposited thin film is subjected to UV exposure treatment for 15~50 s;

[0043] S6, Wet Resin Removal: A wet resist removal process is used, in which the UV-exposed glass tube is immersed in a resist removal reagent for 5-30 minutes to remove the photoresist between the film and the glass tube, thus detaching the film from the glass tube. Subsequently, the detached ultrathin-walled tube is cleaned with anhydrous ethanol and dried to obtain an ultrathin seamless thin-walled tube with an inner diameter of 1-100 mm and a wall thickness of 0.001-0.05 mm.

[0044] Preferably, the substrate is a glass tube; the glass tube includes, but is not limited to, one or more of alumina, sapphire, quartz glass, and other glass components.

[0045] Preferably, the positive photoresist is any one of diazoquinone, polyimide, methacrylic acid, epoxy resin, acrylic acid, etc.

[0046] Preferably, the coating method includes, but is not limited to, dipping, spraying, brushing, dripping, rolling, electrostatic coating, and ultrasonic coating.

[0047] Preferably, the thickness of the photoresist coating on the outer wall of the substrate is 0.001~0.01 mm.

[0048] Preferably, the physical vapor deposition technique is any one of vacuum evaporation deposition, sputtering deposition, or ion plating.

[0049] Preferably, the thin film constituent material is one of various metals, alloys, semiconductors, ceramics, and multilayers or composite materials freely combined from them.

[0050] Preferably, the selected ultraviolet light source is one of g-line, i-line, KrF-line, or ArF-line.

[0051] Preferably, the adhesive remover includes, but is not limited to, organic solvents such as acetone, ethanol, and isopropanol, as well as alkaline inorganic solutions such as sodium hydroxide and potassium hydroxide, or one or more of the following specialized adhesive removers: 1-methyl-2-pyrrolidone, azirethylpyrrolidone, dimethyl sulfoxide, and tetramethylammonium hydroxide.

[0052] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

[0053] The following examples use instruments and equipment conventional in the art. Experimental methods in the following examples, unless otherwise specified, are generally performed under conventional conditions or as recommended by the manufacturer. All raw materials used in the following examples are conventional commercially available products with specifications conventional in the art. In this specification and the following examples, unless otherwise specified, "%" refers to weight percentage, "parts" refers to parts by weight, and "ratio" refers to weight proportion.

[0054] Example 1

[0055] A method for preparing an ultrathin seamless Al thin-walled tube includes the following steps:

[0056] Step 1: Select a quartz glass tube with an outer diameter of 5 mm as a substrate for pretreatment. Immerse the selected quartz glass tube in acetone and anhydrous ethanol in sequence for ultrasonic cleaning for 10 min. After taking it out, rinse it with deionized water and blow it dry with high-purity nitrogen.

[0057] Step 2: The outer wall of the pretreated quartz glass tube is uniformly coated with BP-212 diazonaphthoquinone type UV positive photoresist. The coating is uniformly applied using an ultrasonic coating process with a spraying frequency of 120 kHz and a spraying speed of 0.5 m / s. The thickness of the positive photoresist is 0.005 mm.

[0058] Step 3: Place the quartz glass tube with the positive photoresist evenly coated on it on a constant temperature heating table for soft baking. The temperature is set to 90 ℃ and the time is 50 s to promote the evaporation of residual solvent in the photoresist, so that the photoresist can be cured and hardened, and the adhesion to the substrate can be enhanced.

[0059] Step 4: Using magnetron sputtering ion plating technology, an Al target with a purity of 99.99 wt.% was selected as the sputtering source material. A softened and baked quartz glass tube was placed into the chamber, and a mechanical pump and a molecular pump were used to evacuate the chamber to a vacuum level of 3 × 10⁻⁶. -3Pa was then introduced, followed by the introduction of inert gas Ar (99.99% purity) at a flow rate of 18 sccm. The substrate negative bias was adjusted to 65V, the Al target sputtering power was 420 W, the workpiece holder rotation speed was 5 rpm, and the working gas pressure in the chamber was 1.12 × 10⁻⁶ Pa. -1 Pa, working time is 100 min, after deposition, wait for the chamber temperature to drop to room temperature before taking it out;

[0060] Step 5: Perform ultraviolet exposure treatment on the inner wall of the quartz glass tube with the deposited film, using i-line ultraviolet light as the exposure source, and the exposure time is 30 s;

[0061] Step 6: Immerse the UV-exposed quartz glass tube in an N-methylpyrrolidone solution for 15 minutes to remove the photoresist between the film and the glass tube, and detach the film from the glass tube. Then, take out the detached Al thin-walled tube, clean it with anhydrous ethanol and dry it to obtain an ultra-thin seamless Al thin-walled tube with an inner diameter of 5 mm and a wall thickness of 0.001 mm.

[0062] Example 2

[0063] A method for preparing an ultrathin seamless Cu thin-walled tube includes the following steps:

[0064] Step 1: Select a sapphire tube with an outer diameter of 5 mm as the substrate for pretreatment. Immerse the selected sapphire tube in acetone and anhydrous ethanol in sequence for ultrasonic cleaning for 30 min. After taking it out, rinse it with deionized water and blow it dry with high-purity nitrogen.

[0065] Step 2: The outer wall of the pretreated sapphire tube is uniformly coated with photoresist. BP-212 diazonaphthoquinone type UV positive photoresist is selected and uniformly coated using ultrasonic coating process. The spraying frequency is 120 kHz, the spraying speed is 0.5 m / s, and the thickness of the photoresist is 0.005 mm.

[0066] Step 3: Place the sapphire tube with a uniformly coated positive photoresist onto a constant temperature heating stage for soft baking. The temperature is set to 90 ℃ and the time is 50 s to promote the evaporation of residual solvent in the photoresist, so that the photoresist can be cured and hardened, and the adhesion to the substrate can be enhanced.

[0067] Step 4: Using magnetron sputtering ion plating technology, a Cu target with a purity of 99.99 wt.% was selected as the sputtering source material. A softened sapphire tube was placed into the chamber, and a mechanical pump and a molecular pump were used to evacuate the chamber to a vacuum level of 3 × 10⁻⁶. - 3Pa was then introduced, followed by the introduction of inert gas Ar (99.99% purity) at a flow rate of 18 sccm. The substrate negative bias was adjusted to 65 V, the Cu target sputtering power was 405 W, the workpiece holder rotation speed was 5 rpm, and the working gas pressure in the chamber was 1.12 × 10⁻⁶ Pa. -1 Pa, working time 370 min, after deposition, wait for the chamber temperature to drop to room temperature before removing;

[0068] Step 5: Perform ultraviolet exposure treatment on the inner wall of the sapphire tube with the deposited thin film, using i-line ultraviolet light as the exposure source, and the exposure time is 30 s;

[0069] Step 6: Immerse the UV-exposed sapphire tube in an N-methylpyrrolidone solution for 10 minutes to remove the photoresist between the film and the sapphire tube, and then detach the film from the sapphire tube. Subsequently, remove the detached Cu thin-walled tube, clean it with anhydrous ethanol and dry it to obtain an ultra-thin seamless Cu thin-walled tube with an inner diameter of 5 mm and a wall thickness of 0.03 mm.

[0070] Example 3

[0071] A method for preparing an ultrathin seamless FeCrAl thin-walled tube includes the following steps:

[0072] Step 1: Select a sapphire tube with an outer diameter of 5 mm as the substrate for pretreatment. Immerse the selected sapphire tube in acetone and anhydrous ethanol in sequence for ultrasonic cleaning for 15 min. After taking it out, rinse it with deionized water and blow it dry with high-purity nitrogen.

[0073] Step 2: The outer wall of the pretreated sapphire tube is uniformly coated with photoresist. BP-212 diazonaphthoquinone type UV positive photoresist is selected and uniformly coated using ultrasonic coating process. The spraying frequency is 120 kHz, the spraying speed is 0.5 m / s, and the thickness of the photoresist is 0.005 mm.

[0074] Step 3: Place the sapphire tube with a uniformly coated positive photoresist onto a constant temperature heating stage for soft baking. The temperature is set to 90 ℃ and the time is 50 s to promote the evaporation of residual solvent in the photoresist, so that the photoresist can be cured and hardened, and the adhesion to the substrate can be enhanced.

[0075] Step 4: Using magnetron sputtering ion plating technology, a FeCrAl alloy target with a mass percentage of 94:13:6 wt.% was selected as the sputtering source material. A softened sapphire tube was placed into the chamber, and a mechanical pump and a molecular pump were used to evacuate the chamber to a vacuum level of 3 × 10⁻⁶. -3Pa, then inert gas Ar (purity 99.99%) was introduced at a flow rate of 20 sccm, the substrate negative bias was adjusted to 65 V, the FeCrAl alloy target sputtering power was 900 W, the workpiece holder rotation speed was 5 rpm, and the working gas pressure in the chamber was 1.12 × 10⁻⁶ Pa. -1 Pa, working time 220 min, after deposition, wait for the chamber temperature to drop to room temperature before removing;

[0076] Step 5: Perform ultraviolet exposure treatment on the inner wall of the sapphire tube with the deposited thin film, using i-line ultraviolet light as the exposure source, and the exposure time is 30 s;

[0077] Step 6: Immerse the UV-exposed sapphire tube in an N-methylpyrrolidone solution for 15 minutes to remove the photoresist between the film and the sapphire tube, and then detach the film from the sapphire tube. Subsequently, remove the FeCrAl thin-walled tube after photoresist removal, and then clean and dry it with anhydrous ethanol to obtain an ultra-thin seamless FeCrAl thin-walled tube with an inner diameter of 5 mm and a wall thickness of 0.05 mm.

[0078] Example 4

[0079] A method for preparing an ultrathin seamless AlN thin-walled tube includes the following steps:

[0080] Step 1: Select a quartz glass tube with an outer diameter of 20 mm as a substrate for pretreatment. Immerse the selected quartz glass tube in acetone and anhydrous ethanol in sequence for ultrasonic cleaning for 15 min. After taking it out, rinse it with deionized water and blow it dry with high-purity nitrogen.

[0081] Step 2: The outer wall of the pretreated quartz glass tube is uniformly coated with photoresist. BP-212 diazonaphthoquinone type UV positive photoresist is selected and uniformly coated using ultrasonic coating process. The spraying frequency is 120 kHz, the spraying speed is 0.5 m / s, and the thickness of the photoresist is 0.005 mm.

[0082] Step 3: Place the quartz glass tube with the positive photoresist evenly coated on it on a constant temperature heating table for soft baking. The temperature is set to 90 ℃ and the time is 50 s to promote the evaporation of residual solvent in the photoresist, so that the photoresist can be cured and hardened, and the adhesion to the substrate can be enhanced.

[0083] Step 4: Using magnetron sputtering ion plating technology, an Al target with a purity of 99.99 wt.% was selected as the sputtering source material. A softened and baked quartz glass tube was placed into the chamber, and a mechanical pump and a molecular pump were used to evacuate the chamber to a vacuum level of 3 × 10⁻⁶. -3Pa was then introduced, followed by the introduction of inert gas Ar (99.99% purity) at a flow rate of 20 sccm, and N2 at a flow rate of 30 sccm. The substrate negative bias was adjusted to 65 V, the Al target sputtering power was 420 W, the workpiece holder rotation speed was 5 rpm, and the working gas pressure in the chamber was 1.12 × 10⁻⁶ Pa. -1 Pa, working time is 450 min, after deposition, wait for the chamber temperature to drop to room temperature before taking it out;

[0084] Step 5: Perform ultraviolet exposure treatment on the inner wall of the quartz glass tube with the deposited film, using i-line ultraviolet light as the exposure source, and the exposure time is 30 s;

[0085] Step 6: Immerse the UV-exposed quartz glass tube in an N-methylpyrrolidone solution for 15 minutes to remove the photoresist between the film and the glass tube, and detach the film from the glass tube. Then, take out the AlN thin-walled tube after removing the photoresist, clean it with anhydrous ethanol and dry it to obtain an ultra-thin seamless AlN thin-walled tube with an inner diameter of 20 mm and a wall thickness of 0.03 mm.

[0086] Example 5

[0087] A method for preparing an ultrathin seamless CrN thin-walled tube includes the following steps:

[0088] Step 1: Select a quartz glass tube with an outer diameter of 100 mm as a substrate for pretreatment. Immerse the selected quartz glass tube in acetone and anhydrous ethanol in sequence for ultrasonic cleaning for 15 min. After taking it out, rinse it with deionized water and blow it dry with high-purity nitrogen.

[0089] Step 2: The outer wall of the pretreated quartz glass tube is uniformly coated with photoresist. BP-212 diazonaphthoquinone type UV positive photoresist is selected and uniformly coated using ultrasonic coating process. The spraying frequency is 120 kHz, the spraying speed is 0.5 m / s, and the thickness of the photoresist is 0.005 mm.

[0090] Step 3: Place the quartz glass tube with the positive photoresist evenly coated on it on a constant temperature heating table for soft baking. The temperature is set to 90 ℃ and the time is 50 s to promote the evaporation of residual solvent in the photoresist, so that the photoresist can be cured and hardened, and the adhesion to the substrate can be enhanced.

[0091] Step 4: Using magnetron sputtering ion plating technology, a Cr target with a purity of 99.99 wt.% was selected as the sputtering source material. A softened and baked quartz glass tube was placed into the chamber, and a mechanical pump and a molecular pump were used to evacuate the chamber to a vacuum level of 3 × 10⁻⁶. -3Pa was then introduced, followed by the introduction of inert gas Ar (99.99% purity) at a flow rate of 20 sccm, and N2 at a flow rate of 30 sccm. The substrate negative bias was adjusted to 65 V, the Cr target sputtering power was 900 W, the workpiece holder rotation speed was 5 rpm, and the working gas pressure in the chamber was 1.12 × 10⁻⁶ Pa. -1 Pa, working time is 300 min, after deposition, wait for the chamber temperature to drop to room temperature before taking it out;

[0092] Step 5: Perform ultraviolet exposure treatment on the inner wall of the quartz glass tube with the deposited film, using i-line ultraviolet light as the exposure source, and the exposure time is 30 s;

[0093] Step 6: Immerse the UV-exposed quartz glass tube in an N-methylpyrrolidone solution for 15 minutes to remove the photoresist between the film and the glass tube, and then detach the film from the glass tube. Subsequently, remove the CrN thin-walled tube after photoresist removal, and then clean and dry it with anhydrous ethanol to obtain an ultra-thin seamless CrN thin-walled tube with an inner diameter of 100 mm and a wall thickness of 0.05 mm.

[0094] Example 6

[0095] A method for preparing an ultrathin seamless TiO2 thin-walled tube includes the following steps:

[0096] Step 1: Select a quartz glass tube with an outer diameter of 100 mm as a substrate for pretreatment. Immerse the selected quartz glass tube in acetone and anhydrous ethanol in sequence for ultrasonic cleaning for 15 min. After taking it out, rinse it with deionized water and blow it dry with high-purity nitrogen.

[0097] Step 2: The outer wall of the pretreated quartz glass tube is uniformly coated with photoresist. BP-212 diazonaphthoquinone type UV positive photoresist is selected and uniformly coated using ultrasonic coating process. The spraying frequency is 120 kHz, the spraying speed is 0.5 m / s, and the thickness of the photoresist is 0.005 mm.

[0098] Step 3: Place the quartz glass tube with the positive photoresist evenly coated on it on a constant temperature heating table for soft baking. The temperature is set to 90 ℃ and the time is 50 s to promote the evaporation of residual solvent in the photoresist, so that the photoresist can be cured and hardened, and the adhesion to the substrate can be enhanced.

[0099] Step 4: Using electron beam evaporation deposition technology, TiO2 particles with a purity of 99.99 wt.% were selected as the evaporation source material and placed in a graphite crucible. A softened and baked quartz glass tube was then placed into the chamber. A mechanical pump and a molecular pump were used to evacuate the chamber to a vacuum level of 6 × 10⁻⁶. -4Pa, adjust the preset current to 0.4 A, the preheating current adjustment rate to 0.02 A / min, adjust the spot position to the center of the crucible, adjust the voltage to 8.2 kV, the current to 0.5 A, the beam current to 18 mA, the deposition time to 400 min, and after the deposition is completed, wait for the chamber temperature to drop to room temperature before taking it out;

[0100] Step 5: Perform ultraviolet exposure treatment on the inner wall of the quartz glass tube with the deposited film, using i-line ultraviolet light as the exposure source, and the exposure time is 30 s;

[0101] Step 6: Immerse the UV-exposed quartz glass tube in an N-methylpyrrolidone solution for 15 minutes to remove the photoresist between the film and the glass tube, and then detach the film from the glass tube. Subsequently, remove the detached TiO2 thin-walled tube, clean it with anhydrous ethanol and dry it to obtain an ultra-thin seamless TiO2 thin-walled tube with an inner diameter of 100 mm and a wall thickness of 0.03 mm.

[0102] This invention discloses a method for fabricating ultrathin seamless thin-walled tubes using physical vapor deposition (PVD). This method overcomes the limitations of traditional machining processes on the tube diameter-to-thickness ratio and the difficulty of using thin-walled plates for rolling connections due to excessively thin tube walls. It is applicable to various metals, alloys, semiconductors, ceramics, and multilayer or composite materials freely combined from these materials. The PVD technology in this invention encompasses vacuum evaporation deposition, sputtering deposition, and ion plating. The resulting ultrathin seamless thin-walled tubes have wall thicknesses ranging from 0.001 to 0.05 mm, exhibiting uniform wall structure and thickness, and nanometer-level precision in wall thickness control and surface roughness. The method employed in this invention is simple and energy-efficient, enabling high-precision, large-scale industrial production and facilitating widespread application.

[0103] The above content is only for illustrating the technical concept of the present invention and should not be construed as limiting the scope of protection of the present invention. Any modifications made to the technical solution based on the technical concept proposed in this invention shall fall within the scope of protection of the claims of this invention.

Claims

1. A method for preparing an ultrathin seamless thin-walled tube, characterized in that, Includes the following steps: After pretreatment of the substrate, adhesive is applied to the outer wall of the substrate, followed by soft baking. A thin film was prepared on the outer wall of a substrate after soft baking using physical vapor deposition technology, resulting in a substrate with deposited thin film. The substrate with the deposited thin film is subjected to UV exposure and resist removal treatment in sequence to obtain the detached thin film; After post-processing, the detached film is used to obtain an ultra-thin seamless thin-walled tube. The substrate is a glass tube; the material of the glass tube is alumina, sapphire, or quartz glass. The step of sequentially performing ultraviolet exposure treatment on the substrate with the deposited thin film involves performing ultraviolet exposure treatment on the inner wall of the glass tube with the deposited thin film; the ultraviolet light source used in the ultraviolet exposure treatment is one of g-line, i-line, KrF-line, and ArF-line; The ultraviolet exposure treatment time is 15~50 s.

2. The method for preparing an ultrathin seamless thin-walled tube according to claim 1, characterized in that, The pretreatment steps are as follows: the substrate is ultrasonically cleaned in acetone and anhydrous ethanol solutions for 10-30 min in sequence, and then dried.

3. The method for preparing an ultrathin seamless thin-walled tube according to claim 1, characterized in that, The coating process involves uniformly coating the outer wall of the substrate with a positive photoresist; the positive photoresist is any one of diazoquinone, polyimide, methacrylic acid, epoxy resin, and acrylic resin. The adhesive application method is dip coating, spray coating, brush coating, drop coating, roller coating, electrostatic coating, or ultrasonic coating; the thickness of the adhesive coating is 0.001~0.01 mm.

4. The method for preparing an ultrathin seamless thin-walled tube according to claim 1, characterized in that, The softening process is carried out at a temperature of 90~100 ℃ for 10~60 s.

5. The method for preparing an ultrathin seamless thin-walled tube according to claim 1, characterized in that, The physical vapor deposition technique is any one of vacuum evaporation deposition, sputtering deposition, and ion plating; The material used to prepare the thin film is one of metal, alloy, semiconductor or ceramic; The materials used to prepare the thin film are multilayer or composite materials made of metals, alloys, semiconductors or ceramics in free combination.

6. A method for preparing an ultrathin seamless thin-walled tube according to claim 1, characterized in that, The adhesive removal process is a wet adhesive removal method; the wet adhesive removal time is 5-30 min; the adhesive removal reagent used in the wet adhesive removal is one or more of acetone, ethanol, isopropanol, sodium hydroxide, potassium hydroxide, 1-methyl-2-pyrrolidone, azirethylpyrrolidone, dimethyl sulfoxide and tetramethylammonium hydroxide.

7. A method for preparing an ultrathin seamless thin-walled tube according to claim 1, characterized in that, The outer diameter of the substrate is 1~100 mm.

8. An ultrathin seamless thin-walled tube, characterized in that, It is prepared by the preparation method described in any one of claims 1 to 7.

9. An ultrathin seamless thin-walled tube according to claim 8, characterized in that, The inner diameter of the ultrathin seamless thin-walled tube is 1~100 mm, and the wall thickness is 0.001~0.05 mm.

Images