A peptide thin film evaporation device and method based on physical vapor deposition technology
By designing a peptide thin film evaporation equipment based on physical vapor deposition technology, the problem of easy decomposition of peptide thin films at high temperatures was solved, realizing efficient and controllable peptide thin film preparation and large-scale production.
Patent Information
- Application Number
- CN202310590362.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-24
- Publication Date
- 2025-12-05
- Estimated Expiration
- 2043-05-24
AI Technical Summary
Existing peptide film preparation methods are prone to peptide material decomposition at high temperatures, making it difficult to prepare high-quality and stable peptide films.
A peptide thin film deposition device based on physical vapor deposition technology was designed, including a deposition area module, a gas control module, and a heating module. It adopts a rotary lifting device and a heating module, and achieves efficient deposition of peptide thin films through components such as a vacuum chamber, a sample holder, and heating wires.
It achieves efficient, precise, and controllable peptide film preparation. The equipment has a simple structure, is easy to operate, and is suitable for large-scale production, resulting in improved film quality and stability.
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Figure CN116590669B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to a peptide thin film evaporation device, in particular to a peptide thin film evaporation device and method based on physical vapor deposition technology. BACKGROUND
[0002] Physical vapor deposition is a widely used technology for preparing thin films, its basic principle is to evaporate solid material into gas, and then deposit it on the substrate by vapor deposition to form thin film material. This technology has the advantages of fast deposition speed, uniform deposition, low deposition temperature, etc., and is widely used in semiconductor, optoelectronic, material and other fields.
[0003] Physical vapor deposition technology is a widely used technology in the field of material preparation, which can prepare thin film materials with high quality, high stability and excellent performance. In the field of peptide material preparation, physical vapor deposition technology is also widely used, which can be used to prepare peptide thin films, these thin films have wide application prospects, such as in biomedical, nano-electronics and other fields.
[0004] Peptides are biological macromolecules composed of multiple amino acid residues, with important biological functions and application value. Peptide thin film technology has wide application prospects in the fields of biomedicine, optoelectronics, chemical sensors, etc. For example, the technology of preparing peptide thin films can be used to prepare biosensors and optoelectronic devices for detecting and diagnosing diseases, and can also be used to prepare efficient catalysts and adsorbents, etc. The existing peptide thin film preparation methods mainly include self-assembly, solution spin coating, layer-by-layer self-assembly, etc. Although these methods are simple and easy to operate, the quality and stability of the thin films are poor, which is difficult to meet the requirements of some practical applications.
[0005] However, physical vapor deposition technology faces some unique challenges in the preparation of peptide materials. The molecular structure of peptide materials is relatively complex and is prone to decomposition and degradation at high temperatures. Traditional physical vapor deposition technology needs to be carried out at relatively high temperatures, which makes the peptide material prone to pyrolysis and degradation, thereby reducing the quality and stability of the thin film. Therefore, it is necessary to develop a device and method that can prepare high-quality peptide thin films. SUMMARY
[0006] In order to solve the problems existing in the background art, the present application provides a peptide thin film evaporation device and method based on physical vapor deposition technology.
[0007] The technical scheme adopted by the present application is:
[0008] I. A peptide thin film evaporation device based on physical vapor deposition technology:
[0009] The peptide thin film evaporation equipment comprises a deposition area module, a gas control module and a heating module, the heating module is installed inside the lower side of the deposition area module, and the gas control module is communicated with the inside of the deposition area module; the deposition area module comprises a rotary lifting device and an evaporation deposition device, the rotary lifting device is installed on the top of the evaporation deposition device, and the evaporation deposition device is communicated with the gas control module.
[0010] The evaporation deposition device comprises a vacuum chamber and two sample holders, the bottom end of the rotary lifting device extends to the inside of the chamber and is connected to the top surface of the horizontally arranged fixed plate, the two sample holders are symmetrically installed on the upper side of the inside of the chamber through the fixed plate, the top of the two sample holders is engaged with the lower side of the rotary lifting device, and the heating module is located directly below the two sample holders; the chamber is communicated with the gas control module through the connecting pipes.
[0011] The chamber further comprises two connecting pipes and two flanges, through grooves are formed in the symmetrical two side walls of the chamber, one end of each through groove is connected with the connecting pipe, the other end of the connecting pipe is connected with the flange, a glass window is arranged on the flange to seal the chamber, the glass window is opposite to the sample holder and used for observing the state of the sample holder, the chamber has a three-face rectangular cuboid side wall with an upper opening and a chamber door on the front face, a top plate completely closes the upper opening of the chamber, the chamber door is arranged on the side wall between the two glass windows and is opened or closed through a hinge, the side wall, the top plate and the chamber door of the chamber are made of stainless steel and are polished to improve the corrosion resistance and sealing performance, and the connecting pipes and the flanges are designed to be shock-absorbed to prevent vibration noise while ensuring air tightness.
[0012] The sample holder comprises a sample holder, a sample holder seat, a conductive ring, a ceramic ring, a circular cover, a large cylinder, a large bottom ring, a long cylinder, a small bottom ring and a self-rotation gear, the sample holder seat, the conductive ring, the ceramic ring, the circular cover, the large cylinder, the large bottom ring, the long cylinder, the small bottom ring and the self-rotation gear are arranged in a horizontal concentric manner from bottom to top, the large cylinder and the large bottom ring are arranged on the bottom surface and the top surface of the fixed plate respectively, the large bottom ring is sleeved on the outer side of the long cylinder, the bottom end of the long cylinder penetrates through the large bottom ring and the fixed plate and is connected with the top end of the large cylinder, the side surface of the sample holder seat is provided with an installation groove facing the inside of the sample holder seat, the sample holder is arranged in the installation groove of the sample holder seat in a concentric manner, the self-rotation gear is engaged with the lower part of the rotary lifting device, the bottom of the sample holder seat is provided with a circular through groove penetrating the installation groove, the bottom surface of the sample holder is opposite to the circular through groove, and the heating module is located directly below the two circular through grooves.
[0013] The sample holder is disc-shaped, and the sample holder seat with a hollow structure can clasp the sample holder with a cylindrical handle from below, and the sample holder has good dimensional accuracy and surface flatness. The conductive ring and the ceramic ring are used for biasing and insulation, respectively, to improve the quality of the deposited layer; the conductive ring, the ceramic ring and the round cover are fixedly connected with the sample holder seat through bolts and nuts; the large cylinder, the large bottom ring, the long cylinder and the small bottom ring are used for connecting the self-rotation gear with the sample holder part below. The diameter of the large cylinder is larger than that of the long cylinder, and the height of the large cylinder is smaller than that of the long cylinder.
[0014] The rotating lifting device comprises a rotating part and a lifting part, the rotating part comprises a sample from tooth, a motor support plate, a self-rotation motor, a self-rotation main tooth and a main shaft, the main shaft is vertically arranged, the lower end of the main shaft is connected to the center of the top surface of the fixed plate, the sample from tooth is sleeved on the lower part of the main shaft, the upper end and the lower end of the sample from tooth are each provided with a horizontal gear and are located outside and inside the chamber respectively, the gear at the lower end of the sample from tooth and the self-rotation gears of the two sample holders are in mesh with each other; the self-rotation motor and the self-rotation main tooth are installed on the outer top surface of the chamber through the motor support plate, the self-rotation motor is located directly above the self-rotation main tooth, the self-rotation main tooth is horizontally arranged, the output shaft of the self-rotation motor is synchronously connected to the center of the self-rotation main tooth, the gear at the upper end of the sample from tooth is located on the motor support plate and is in mesh with the self-rotation main tooth.
[0015] In the vacuum chamber, the two groups of sample holders are distributed left and right symmetrically, and the two self-rotation gears realize synchronous movement through the sample from tooth at the same horizontal plane of the symmetry center. The self-rotation movement of the sample holder is directly transmitted to the self-rotation main tooth by the self-rotation motor on the motor support plate after being started, and then the two self-rotation gears are driven to rotate by the sample from tooth, and the self-rotation of the sample holder is realized. The sample from tooth is an integral tooth shaft with two gears, the lower gear is matched with the two self-rotation gears as described above, and the upper gear is matched with the self-rotation main tooth. The rotating lifting device is also provided with a gear anti-pollution plate to prevent the upper teeth of the self-rotation main tooth and the sample from tooth from being polluted by the outside.
[0016] The lifting part comprises a stepping motor, a small pulley, a conveyor belt, a large pulley, a transmission screw, a transmission nut, a moving connecting plate, an upper corrugated pipe flange, a corrugated pipe, a loose sleeve flange, a lower fixed plate, an upper fixed plate, a supporting guide shaft, a limiting block and a mounting plate; the upper end of the main shaft is connected to the bottom end of the corrugated pipe; the upper corrugated pipe flange is sleeved on the upper end of the corrugated pipe; the loose sleeve flange is sleeved on the connection between the corrugated pipe and the main shaft; the outer side of the loose sleeve flange is connected to one side of the horizontally arranged lower fixed plate; the bottom surface of the other side of the lower fixed plate away from the main shaft is connected to the top surface of one side of the horizontally arranged mounting plate; the stepping motor is installed on the top surface of the other side of the mounting plate; the output shaft of the stepping motor is vertically downwardly provided through the mounting plate and is synchronously connected to the center of the small pulley; the upper fixed plate is horizontally arranged above the lower fixed plate and is installed in front of the lower fixed plate; the bottom end of the supporting guide shaft is provided through the lower fixed plate and is connected to the top surface of the mounting plate; the vertically arranged transmission screw is further installed between the lower fixed plate and the upper fixed plate; the bottom end of the transmission screw is sequentially provided through the lower fixed plate and the mounting plate and is synchronously connected to the center of the large pulley; the large pulley and the small pulley are located at the same height; the small pulley is drivingly connected to the large pulley through the conveyor belt; the transmission nut is threadedly sleeved on the transmission screw; the transmission nut is connected to one side of the horizontally arranged moving connecting plate; the other side of the moving connecting plate is supported on the bottom surface of the upper corrugated pipe flange; the limiting block is further arranged on the transmission screw and the supporting guide shaft and is located between the transmission nut and the lower fixed plate; and the limiting block defines the limiting position of the downward movement of the transmission nut.
[0017] The lifting part further comprises a scale which is vertically installed between the lower fixed plate and the upper fixed plate and is close to the transmission screw; the side surface of one side of the moving connecting plate close to the scale is provided with a horizontal pointer; and the end of the pointer points to the scale.
[0018] The corrugated pipe comprises two corrugated pipe connectors, two corrugated pipe joints and corrugated sheets; the two corrugated pipe connectors are vertically arranged in coaxial arrangement on the upper and lower sides of the corrugated sheets; the two ends of the corrugated sheets are connected to the two corrugated pipe connectors through the two corrugated pipe joints; and the expansion direction of the corrugated sheets is the vertical direction; the upper corrugated pipe flange is sleeved on the upper end of the upper corrugated pipe connector; the lower end of the lower corrugated pipe connector is coaxially connected to the upper end of the main shaft; and the loose sleeve flange is sleeved on the connection between the lower end of the lower corrugated pipe connector and the upper end of the main shaft. The corrugated pipe is used for buffering when the device is lifted.
[0019] The stepping motor is used to drive the sample holder to move in the z-axis. After the stepping motor is started, the motor shaft drives the small pulley to rotate, and the transmission belt further transmits the movement to the large pulley. The large pulley is connected with the transmission screw and the transmission nut to convert the rotary motion into linear motion. The transmission nut is tightly connected with the moving connecting plate, and the movement of the transmission nut can make the moving connecting plate and the flange on the corrugated pipe move together, so as to drive the corrugated pipe to realize the expansion and contraction in the z-axis, and further drive the main shaft to realize the lifting movement in the z-axis.
[0020] The deposition area module is used to provide a thin film deposition environment, the gas control module is used to control the gas pressure of the deposition area module, and the heating module is used to heat the target material, control the heating gradient and the deposition time. The vacuum chamber of the deposition area module is used to maintain a high vacuum environment to ensure that the evaporation material is not oxidized and contaminated at high temperature. The vacuum chamber is connected through a flange and a sealing element to ensure the stability of the vacuum degree and the sealing property. The sample holder is used to fix the substrate on the carrier of the deposition area, so that the substrate can be uniformly heated and cooled. The sample holder is made of stainless steel. The sample holder can realize self-rotation and Z-axis movement. In order to evaporate the peptide powder, the minimum target distance, i.e. the distance between the target material and the substrate, can reach 10 mm. The deposition area module further comprises a vacuum measurement module for measuring and displaying the vacuum parameters in the thin film deposition cavity, and a visual window module for the operator to observe whether the target material in the cavity is completely evaporated.
[0021] The heating module comprises two heaters, each of which comprises an evaporation dish, a boron nitride sheet, a heating wire, a uniform heating plate, two ceramic tubes, a heating upper shielding cylinder, an inner heating shielding cylinder, an outer heating shielding cylinder, a heat insulation plate and a heating outer shielding cylinder. The uniform heating plate is a stepped cylindrical hollow cylinder structure. The inner part of the upper cylinder of the uniform heating plate is provided with a rounded table groove. The inner part of the lower cylinder of the uniform heating plate is provided with a cylindrical groove. The outer diameter of the upper cylinder of the uniform heating plate is larger than that of the lower cylinder. The evaporation dish is a rounded table disc. The evaporation dish is placed in the rounded table groove of the upper cylinder of the uniform heating plate. The evaporation dish is directly below the circular through groove of the sample holder of each sample holder. The boron nitride sheet is horizontally installed in the cylindrical groove of the lower cylinder of the uniform heating plate. The heat insulation plate is horizontally installed and covers the bottom end of the uniform heating plate. The boron nitride sheet serves as a main heating device and is directly placed below the evaporation dish. The heat can be quickly and uniformly transmitted to the sample surface through the uniform heating plate. The heating wire is spirally wound on the outer coil plate surface of the boron nitride sheet. The two ends of the heating wire pass through the heat insulation plate downward. The two ends of the heating wire are sleeved with ceramic tubes. The heating wire can improve the heating rate and sublimation quality by releasing a large amount of heat energy to the environment. The ceramic tubes can prevent excessive loss by wrapping the pins at the two ends of the heating wire. The outer side of the lower cylinder of the uniform heating plate is sequentially sleeved with the inner heating shielding cylinder and the outer heating shielding cylinder. The upper end of the heating upper shielding cylinder is sleeved on the outer side of the outer heating shielding cylinder. The heating outer shielding cylinder is sleeved on the outer side of the upper cylinder of the uniform heating plate and the heating upper shielding cylinder. The heating upper shielding cylinder is installed on the inner lower side of the chamber through the installation support. The side surface of the upper end of the lower cylinder of the uniform heating plate, the inner heating shielding cylinder, the outer heating shielding cylinder and the heating upper shielding cylinder is circumferentially and uniformly spaced with a plurality of fixing holes. A plurality of screws pass through the fixing holes in sequence and abut against the side periphery of the boron nitride sheet to fix the boron nitride sheet in the cylindrical groove, thereby ensuring the rapid sublimation and high-quality deposition of the deposited sample substrate. The heating wire is made of metal tantalum material. The diameter of the heating wire is 0.3 mm. The heating wire is uniformly wound on the uniform heating sheet in the form of a spring ring.
[0022] The heating source is used to quickly and uniformly heat the raw material to its evaporation temperature. The heat insulation module comprises ceramic tubes, a heating outer shielding cylinder, a heating outer shielding cylinder, an outer heating shielding cylinder and an inner heating shielding cylinder, which are used to prevent the high-temperature heating from affecting the deposit. The temperature control system is used to monitor and control the temperature of the heating source, to ensure that the evaporation temperature of the raw material is maintained stable, and to display the temperature value in real time. The evaporation dish is used to load the solid evaporation material therein, to evaporate the solid evaporation material by heating and to deposit the solid evaporation material on the substrate surface.
[0023] The gas control module comprises a gas control box, a gas releasing passage and a gas pumping passage. The gas releasing passage comprises a nitrogen cylinder, a flow meter, a pressure reducing valve, a gas releasing valve and a gas releasing pipe. The nitrogen cylinder is connected to the chamber of the deposition area module through the gas releasing pipe and a connecting pipe. The pressure reducing valve and the gas releasing valve are arranged on the gas releasing pipe between the nitrogen cylinder and the connecting pipe. The flow meter is arranged on the gas releasing pipe between the nitrogen cylinder and the pressure reducing valve. The nitrogen cylinder, the flow meter and the pressure reducing valve are located outside the gas control box, and the gas releasing valve is located inside the gas control box. The nitrogen cylinder is used to provide the required nitrogen source in the vacuum chamber. The nitrogen cylinder is used as a carrier for storing gas in the gas releasing passage, and high-purity nitrogen is filled in the nitrogen cylinder to ensure that the deposition material is not affected by pollution. During the deposition process, nitrogen is released from the nitrogen cylinder to supply the inside of the vacuum chamber as required. The pressure reducing valve is used to better control the flow and pressure of nitrogen. When the process needs to release gas, the nitrogen is transported into the vacuum chamber through the connecting pipe and the loose flange pipe under the condition that the gas releasing valve and the pressure reducing valve are opened at the same time.
[0024] The gas pumping passage comprises a mechanical pump, a bypass valve, a solenoid valve, a molecular pump, a gate valve and two gas pumping pipes. The mechanical pump and the molecular pump are connected through one gas pumping pipe connected to the outside atmosphere. The molecular pump and one gas pumping pipe of the gas control box are provided with the solenoid valve. The gate valve is arranged on one gas pumping pipe between the mechanical pump and the molecular pump. One end of the other gas pumping pipe is connected to one gas pumping pipe between the mechanical pump and the gate valve. The other end of the other gas pumping pipe is connected to the outside atmosphere. The bypass valve is arranged on the other gas pumping pipe. The gas pumping passage is located in the gas control box.
[0025] The gas pumping passage is used to pump out the gas in the vacuum chamber to ensure the high-pressure environment required during the experiment. Under different working conditions, two different modes are adopted: high-pressure and low-pressure modes. When the atmosphere needs to be quickly pumped out in the low-pressure state, the mechanical pump and the bypass valve can be opened. The mechanical pump can quickly and effectively pump the atmosphere into the equipment. When the pressure in the vacuum chamber reaches a certain value, the solenoid valve and the mechanical pump are opened, and the bypass valve is closed. At this time, the mechanical pump and the bypass valve jointly complete the pretreatment and primary pumping of the gas. Then, the solenoid valve starts to work to inject the gas into the molecular pump. In order to better protect the molecular pump, a gate valve is arranged above the molecular pump to balance the gas pressure and protect the molecular pump. Under the control of the bypass valve and the gate valve, the gas pumping passage can quickly and stably pump out the gas to ensure that the gas pressure in the chamber is stably controlled below 4×10 -4 Pa to meet the requirements of normal operation of the equipment. The gas control box is firmly supported to the chamber through several branch pipes.
[0026] The mechanical pump and the bypass valve of the gas control module are used to avoid the vacuum chamber module from being polluted by other gases and to preliminarily reduce the gas pressure in the chamber. The molecular pump, the electromagnetic valve and the gate valve are used to avoid the vacuum chamber from being polluted by other gases, to reduce the gas pressure in the chamber and to further reduce the gas pressure so that the chamber reaches a high vacuum degree; the gas releasing valve is used to release gas into the chamber after the evaporation is completed so as to balance the gas pressure inside and outside the chamber.
[0027] II. A method for evaporation of a peptide film evaporation device:
[0028] The method comprises the following steps:
[0029] Step one: two substrates are respectively pasted on the center of the bottom surface of two sample holders of the deposition area module and are opposite to the circular through-slots of the respective sample holder seats, and the target materials are placed on the two evaporation pans of the heating module.
[0030] Step two: the output shaft of the stepping motor of the lifting part of the rotary lifting device of the deposition area module rotates to sequentially drive the small pulley, the transmission belt, the large pulley and the transmission lead screw to rotate around the respective axes, drive the transmission nut to move along the length direction of the transmission lead screw, thereby drive the moving connecting plate to drive the upper flange of the bellows so that the rotary part as a whole moves the two sample holder frames of the evaporation deposition device along the length direction of the transmission lead screw through the fixed plate, until the pointer on the moving connecting plate points to the preset mark on the scale, so that the distance between each substrate and the respective opposite target material is equal to the preset distance, and the stepping motor is stopped; the distance between the target material and the substrate can be as small as 10 mm.
[0031] Step three: the mechanical pump and the bypass valve of the gas control module are opened, the atmospheric air is rapidly pumped out by the mechanical pump until the gas pressure in the gas control box reaches 20 Pa; the bypass valve is closed, the electromagnetic valve, the molecular pump and the gate valve are opened, and the gas pressure in the chamber is reduced to 4x10 -4 Pa by the molecular pump.
[0032] Step four: the heating wire is heated, and at the same time, the output shaft of the self-rotation motor of the rotary part of the rotary lifting device of the deposition area module rotates to sequentially drive the self-rotation main tooth, the sample from tooth and the self-rotation gear of the two sample holder frames to rotate around the center axis thereof, thereby driving the two sample holder frames to rotate around the center axis of the respective self-rotation gear, and the target material is rotated and heated at 400℃ for 10 min by the heat radiation of the heating wire, and the target material sublimates and deposits on the substrate bottom surface to form a thin film.
[0033] Step five: the nitrogen cylinder, the pressure reducing valve and the gas releasing valve of the gas control module are opened, the nitrogen cylinder injects nitrogen with a preset flow rate into the chamber through the flowmeter until the gas pressure in the chamber is equal to the atmospheric pressure, and the chamber is opened to take out the peptide film evaporated on the substrate bottom surface.
[0034] The base is glass, silicon wafer, metal or polymer substrate; the target material is made of peptide powder material, and the deposition amount of the target material is between 0.1 mg and 150.0 mg.
[0035] The beneficial effects of the present application are:
[0036] The device can efficiently, accurately and controllably prepare the peptide thin film, the peptide thin film prepared by the self-assembly method has high controllability and repeatability, the structure of the device is simple, the preparation process is easy to operate, and the device can mass-produce the peptide thin film structure. BRIEF DESCRIPTION OF DRAWINGS
[0037] Figure 1 is a structural schematic diagram of a physical vapor deposition peptide thin film evaporation equipment adopted by the embodiment of the present application;
[0038] Figure 2 is a structural schematic diagram of a deposition area module of the inventive device;
[0039] Figure 3 is an enlarged structural schematic diagram of a base lifting part in the deposition area module of the inventive device;
[0040] Figure 4 is a structural schematic diagram of a gas control module of the inventive device;
[0041] Figure 5 is an assembly explosion schematic diagram of a heating module of the inventive device;
[0042] Figure 6 is an enlarged structural schematic diagram of a heating wire and a uniform heating sheet of the heating module of the inventive device;
[0043] In the diagram: 10. Deposition area module; 101. Chamber; 101a. Side wall; 101c. Chamber door; 102. Connecting pipe; 103. Flange; 104. Sample holder; 105. Sample holder base; 106. Conductive ring; 107. Ceramic ring; 108. Round cover; 109. Large cylinder; 110. Large bottom ring; 111. Long cylinder; 112. Small bottom ring; 113. Rotating gear; 114. Sample starting gear, 115, motor support plate, 116, self-rotating motor, 117, main self-rotating gear, 118, gear anti-fouling plate, 119, stepper motor, 120, small pulley, 121, conveyor belt, 122, large pulley, 123, transmission screw, 124, transmission nut, 125, moving connecting plate, 126, bellows upper flange, 127, bellows, 127a, bellows connecting pipe, 127b 127c Corrugated pipe fitting, 128 Corrugated sheet, 129 Loose flange, 130 Lower fixing plate, 131 Upper fixing plate, 132 Support guide shaft, 133 Scale, 134 Limit block, 135 Main shaft, 136 Fixing plate, 20 Gas control module, 201 Nitrogen cylinder, 202 Flow meter, 203 Pressure reducing valve, 204 Venting valve, 205 Connecting pipe, 206 Mechanical pump, 207 Bypass valve, 208 Solenoid valve, 209 Gate valve, 210 Molecular pump, 30 Heating module, 301 Evaporating dish, 302 Boron nitride sheet, 303 Heating wire, 304 Heat equalizing plate, 305 Ceramic tube, 306 Upper heating shield, 307 Inner heating shield, 308 Outer heating shield, 309 Heat insulation plate, 310 Outer heating shield. Detailed Implementation
[0044] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
[0045] like Figure 1 As shown, the peptide thin film evaporation equipment of the present invention includes a deposition area module 10, a gas control module 20, and a heating module 30. The heating module 30 is installed inside the lower side of the deposition area module 10, and the gas control module 20 is connected to the interior of the deposition area module 10. The deposition area module 10 includes a rotary lifting device and an evaporation deposition device. The rotary lifting device is installed on the top of the evaporation deposition device, and the evaporation deposition device is connected to the gas control module 20.
[0046] like Figure 2 As shown, the vapor deposition apparatus includes a vacuum chamber 101 and two sample holders. The bottom end of the rotary lifting device extends into the interior of the chamber 101 and is connected to the top surface of a horizontally arranged fixed plate 135. The two sample holders are symmetrically installed on the upper side of the interior of the chamber 101 through the fixed plate 135. The tops of the two sample holders and the lower sides of the rotary lifting device are engaged. The heating module 30 is located directly below the two sample holders. The chamber 101 is connected to the gas control module 20 through the pipe 205.
[0047] The chamber 101 further comprises two connecting pipes 102 and two flanges 103, and the symmetrical two side walls of the chamber 101 are provided with through grooves, the outer side of each groove is connected to one end of the connecting pipe 102, the other end of the connecting pipe 102 is connected to the flange 103, and the flange 103 is provided with a glass window to seal the chamber 101, the glass window is opposite to the sample holder, and is used for observing the state of the sample holder. The chamber 101 has a three-sided rectangular sidewall 101a with an upper opening and a front chamber door 101b, a top plate 101c completely closing the upper opening of the chamber 101, the chamber door 101b is located on the sidewall 101a between the two glass windows and is opened and closed through a hinge. The sidewall 101a, the top plate 101c and the chamber door 101b of the chamber 101 are all made of stainless steel and are polished to improve corrosion resistance and sealing performance; the connecting pipe 102 and the flange 103 are designed to be shock-absorbing, which can effectively prevent vibration noise while ensuring air tightness.
[0048] The sample holder comprises a sample holder 104, a sample holder seat 105, a conductive ring 106, a ceramic ring 107, a circular cover 108, a large cylinder 109, a large bottom ring 110, a long cylinder 111, a small bottom ring 112 and a self-rotation gear 113, the sample holder seat 105, the conductive ring 106, the ceramic ring 107, the circular cover 108, the large cylinder 109, the large bottom ring 110, the long cylinder 111, the small bottom ring 112 and the self-rotation gear 113 are arranged in sequence from bottom to top and are horizontally concentric, the large cylinder 109 and the large bottom ring 110 are arranged on the bottom surface and the top surface of the fixed plate 135 respectively, the large bottom ring 110 is sleeved on the outer side of the long cylinder 111, the bottom end of the long cylinder 111 penetrates through the large bottom ring 110 and the fixed plate 135 and is connected to the top end of the large cylinder 109; the side surface of the sample holder seat 105 is provided with a mounting groove facing the inside of the sample holder seat 105, the sample holder 104 is arranged concentrically in the mounting groove of the sample holder seat 105; the self-rotation gear 113 is engaged with the lower part of the rotary lifting device; the bottom of the sample holder seat 105 is provided with a circular through groove penetrating the mounting groove, and the bottom center of the sample holder 104 is opposite to the circular through groove, and the heating module 30 is located below the two circular through grooves.
[0049] The sample holder is disc-shaped, the sample holder seat 105 with a hollow structure can clasp the sample holder 104 with a cylindrical handle from below, and the sample holder 104 has good dimensional accuracy and surface flatness. The conductive ring 106 and the ceramic ring 107 are respectively used for applying bias and insulation to improve the quality of the deposited layer; the conductive ring 106, the ceramic ring 107 and the circular cover 108 are fixedly connected to the sample holder seat 105 through bolts and nuts; the large cylinder 109, the large bottom ring 110, the long cylinder 111 and the small bottom ring 112 are used for connecting the self-rotation gear 113 and the sample holder part below. The diameter of the large cylinder 109 is greater than that of the long cylinder 111, and the height of the large cylinder 109 is less than that of the long cylinder 111.
[0050] like Figure 3 As shown, the rotary lifting device includes a rotating part and a lifting part. The rotating part includes a sample follower gear 114, a motor support plate 115, a self-rotating motor 116, a self-rotating main gear 117, and a main shaft 134. The main shaft 134 is vertically arranged, and its lower end is connected to the center of the top surface of the fixed plate 135. The sample follower gear 114 is fitted onto the lower part of the main shaft 134. A horizontal gear is provided at both the upper and lower ends of the sample follower gear 114, located outside and inside the chamber 101, respectively. The sample follower gear... The gear at the lower end of tooth 114 meshes with the rotating gears 113 of the two sample holders; the rotating motor 116 and the rotating main gear 117 are mounted on the outer top surface of the chamber 101 through the motor support plate 115. The rotating motor 116 is located directly above the rotating main gear 117, which is horizontally arranged. The output shaft of the rotating motor 116 is synchronously connected to the center of the rotating main gear 117. The sample is fed from the gear at the upper end of tooth 114, which is located on the motor support plate 115 and meshes with the rotating main gear 117.
[0051] Inside the vacuum chamber 101, two sets of sample holders are symmetrically distributed left and right. Two rotating gears 113 move synchronously via sample trailing gears 114 located on the same horizontal plane at the center of symmetry. The rotation of the sample holders is initiated by a rotating motor 116 on the motor support plate 115, which directly transmits the rotation to the main rotating gear 117. This, in turn, drives the two rotating gears 113 to rotate via the sample trailing gears 114, thus achieving the rotation of the sample holders. The sample trailing gear 114 is an integrally formed gear shaft with two gears. The lower gear meshes with the two rotating gears 113 as described above, while the upper gear meshes with the main rotating gear 117. The rotating lifting device also includes a gear anti-contamination plate 118 to prevent external contamination of the upper teeth of the main rotating gear 117 and the sample trailing gear 114.
[0052] The lifting part comprises a stepping motor 119, a small pulley 120, a transmission belt 121, a large pulley 122, a transmission screw 123, a transmission nut 124, a moving link plate 125, an upper corrugated pipe flange 126, a corrugated pipe 127, a loose sleeve flange 128, a lower fixed plate 129, an upper fixed plate 130, a support guide shaft 131, a limiting block 133 and a mounting plate. The upper end of the main shaft 134 is connected to the bottom end of the corrugated pipe 127. The upper corrugated pipe flange 126 is sleeved on the upper end of the corrugated pipe 127. The loose sleeve flange 128 is sleeved on the connection between the corrugated pipe 127 and the main shaft 134. The outer side of the loose sleeve flange 128 is connected to one side of the horizontally arranged lower fixed plate 129. The bottom surface of the other side of the lower fixed plate 129 away from the main shaft 134 is connected to the top surface of one side of the horizontally arranged mounting plate. The stepping motor 119 is installed on the top surface of the other side of the mounting plate. The output shaft of the stepping motor 119 is vertically downwardly threaded through the mounting plate and synchronously connected to the center of the small pulley 120. The upper fixed plate 130 is horizontally opposite to the lower fixed plate 129 and is installed above the lower fixed plate 129 through the vertically arranged support guide shaft 131. The bottom end of the support guide shaft 131 is threaded through the lower fixed plate 129 and connected to the top surface of the mounting plate. The vertically arranged transmission screw 123 is further installed between the lower fixed plate 129 and the upper fixed plate 130. The bottom end of the transmission screw 123 is threaded through the lower fixed plate 129 and the mounting plate in sequence and synchronously connected to the center of the large pulley 122. The large pulley 122 and the small pulley 120 are located at the same height. The small pulley 120 is drivingly connected to the large pulley 122 through the transmission belt 121. The transmission nut 124 is threadedly sleeved on the transmission screw 123. The transmission nut 124 is connected to one side of the horizontally arranged moving link plate 125. The other side of the moving link plate 125 is supported on the bottom surface of the upper corrugated pipe flange 126. The transmission screw 123 and the support guide shaft 131 are further provided with the limiting block 133. The limiting block 133 is located between the transmission nut 124 and the lower fixed plate 129. The limiting block 133 defines the limiting position of the downward movement of the transmission nut 124.
[0053] The lifting part further comprises a scale 132. The scale 132 is vertically installed between the lower fixed plate 129 and the upper fixed plate 130 and close to the transmission screw 123. A horizontal pointer is arranged on the side surface of one side of the moving link plate 125 close to the scale 132. The end of the pointer points to the scale of the scale 132. The height of the lifting of the sample holder is indicated by the pointer on the moving link plate 125 at the corresponding scale of the scale 132.
[0054] The bellows 127 comprises two bellows connecting pipes 127a, two bellows joints 127b and a bellows sheet 127c. The two bellows connecting pipes 127a are arranged vertically and coaxially on the upper and lower sides of the bellows sheet 127c. The two ends of the bellows sheet 127c are connected to the two bellows connecting pipes 127a through the two bellows joints 127b. The expansion direction of the bellows sheet 127c is vertical. The upper flange 126 is sleeved on the upper end of the upper bellows connecting pipe 127a. The lower end of the lower bellows connecting pipe 127a is coaxially connected to the upper end of the main shaft 134. The loose sleeve flange 128 is sleeved on the connection between the lower end of the lower bellows connecting pipe 127a and the upper end of the main shaft 134. The bellows 127 is used for buffering during lifting of the device.
[0055] The stepping motor 119 is used to drive the sample holder to move vertically along the z-axis. After the stepping motor 119 is started, the motor shaft drives the small pulley 120 to rotate. The transmission belt 121 further transmits the movement to the large pulley 122. The large pulley 122 is connected to the transmission screw rod 123 and the transmission nut 124, and converts the rotary motion into linear motion. The transmission nut is tightly connected to the moving connecting plate 125, and the movement of the transmission nut can drive the moving connecting plate 125 to move together with the upper flange 126 of the bellows, so as to drive the bellows 127 to expand and contract in the z-direction, and further drive the main shaft to move vertically along the z-axis.
[0056] The deposition area module 10 is used to provide a thin film deposition environment. The gas control module 20 is used to control the gas pressure of the deposition area module. The heating module 30 is used to heat the target material and control the heating gradient and deposition time. The vacuum chamber 101 of the deposition area module 10 is used to maintain a high vacuum environment to ensure that the evaporation material is not oxidized and contaminated at high temperature. The vacuum chamber 101 is connected through a flange and a sealing element to ensure the stability of the vacuum degree and the sealing property. The sample holder is used to fix the substrate on the carrier of the deposition area, so that the substrate can be uniformly heated and cooled. The sample holder is made of stainless steel. The sample holder can rotate and move vertically along the z-axis. The minimum target distance, i.e. the distance between the target material and the substrate, can reach 10 mm to be suitable for evaporation of peptide powder. The deposition area module 10 further comprises a vacuum measurement module for measuring and displaying the vacuum parameters in the thin film deposition cavity, and a visual window module for allowing an operator to observe whether the target material in the cavity is completely evaporated.
[0057] As Figure 5 and Figure 6As shown, the heating module 30 comprises two heaters, each of which comprises an evaporation dish 301, a boron nitride sheet 302, a heating wire 303, a uniform heating plate 304, two ceramic tubes 305, a heating upper shielding cylinder 306, an inner heating shielding cylinder 307, an outer heating shielding cylinder 308, a heat insulation plate 309, and a heating outer shielding cylinder 310. The uniform heating plate 304 is a stepped cylindrical hollow cylinder structure. The upper cylinder of the uniform heating plate 304 is internally provided with a rounded table groove, and the lower cylinder of the uniform heating plate 304 is internally provided with a cylindrical groove. The outer diameter of the upper cylinder of the uniform heating plate 304 is greater than that of the lower cylinder. The evaporation dish 301 is a rounded table disc, which is placed in the rounded table groove of the upper cylinder of the uniform heating plate 304, directly opposite and below the circular through groove of the sample holder 105 of the respective sample holder. The boron nitride sheet 302 is horizontally installed in the cylindrical groove of the lower cylinder of the uniform heating plate 304, and the heat insulation plate 309 is horizontally installed and covers the bottom end of the uniform heating plate 304. The boron nitride sheet 302 serves as a main heating device, is directly placed below the evaporation dish 301, and ensures that heat can be quickly and uniformly transmitted to the sample surface through the uniform heating plate 304. The heating wire 303 is spirally wound on the outer coil surface of the boron nitride sheet 302. The two ends of the heating wire 303 pass through the heat insulation plate 309 downward. The two ends of the heating wire 303 are sleeved with the ceramic tubes 305. The heating wire 303 can improve the heating rate and sublimation quality by releasing a large amount of heat energy to the environment. The ceramic tubes 305 wrapped at the pins of the two ends of the heating wire 303 can prevent excessive loss of heat dissipation. The outer side of the lower cylinder of the uniform heating plate 304 is sequentially sleeved with the inner heating shielding cylinder 307 and the outer heating shielding cylinder 308. The upper end of the heating upper shielding cylinder 306 is sleeved on the outer side of the outer heating shielding cylinder 308. The heating outer shielding cylinder 310 is sleeved on the outer side of the upper cylinder of the uniform heating plate 304 and the heating upper shielding cylinder 306. The heating upper shielding cylinder 306 is installed on the inside of the lower side of the cavity 101 through the installation bracket. The side surface of the upper end of the lower cylinder of the uniform heating plate 304, the inner heating shielding cylinder 307, the outer heating shielding cylinder 308, and the heating upper shielding cylinder 306 is circumferentially and uniformly spaced with a plurality of fixed holes. A plurality of screws pass through the respective fixed holes and abut against the side periphery of the boron nitride sheet 302 to fix the boron nitride sheet 302 in the cylindrical groove, thereby ensuring the rapid sublimation and high-quality deposition of the deposited sample substrate sheet. The heating wire is made of metal tantalum material, and the diameter of the heating wire is 0.3 mm, which is uniformly wound on the uniform heating sheet in the form of a spring ring.
[0058] The heating source is used to heat the raw material quickly and uniformly to its evaporation temperature; the heat insulation module includes ceramic tube 305, heating outer shielding cylinder 1, heating outer shielding cylinder 2, outer heating shielding cylinder 308, and inner heating shielding cylinder 307, which are used to prevent high-temperature heating from affecting the deposit; and the temperature control system is used to monitor and control the temperature of the heating source, ensure that the evaporation temperature of the raw material is maintained stable, and display the temperature value in real time. The evaporation dish is used to load the solid evaporation material therein, evaporate it by heating, and deposit it on the substrate surface.
[0059] As shown in Figure 4 The gas control module 20 includes a gas control box, a gas release path, and a gas extraction path. The gas release path includes a nitrogen cylinder 201, a flow meter 202, a pressure reducing valve 203, a gas release valve 204, and a gas release pipe. The nitrogen cylinder 201 is connected to the chamber 101 of the deposition area module 10 through the gas release pipe and a connecting pipe 205. The pressure reducing valve 203 and the gas release valve 204 are arranged on the gas release pipe between the nitrogen cylinder 201 and the connecting pipe 205. The flow meter 202 is arranged on the gas release pipe between the nitrogen cylinder 201 and the pressure reducing valve 203. The nitrogen cylinder 201, the flow meter 202, and the pressure reducing valve 203 are located outside the gas control box, and the gas release valve 204 is located inside the gas control box. The nitrogen cylinder 201 is used to provide the required nitrogen source to the vacuum chamber 101. The nitrogen cylinder 201 serves as a carrier for storing gas in the gas release path and contains high-purity nitrogen to ensure that the deposition material is not contaminated. During the deposition process, nitrogen is released from the nitrogen cylinder as needed to supply the inside of the vacuum chamber. The pressure reducing valve 203 is used to better control the flow and pressure of nitrogen. When the process needs to release gas, the nitrogen is transported into the vacuum chamber 101 through the connecting pipe 205 and other pipelines such as a loose flange when the gas release valve 204 and the pressure reducing valve 203 are opened at the same time.
[0060] The gas extraction path includes a mechanical pump 206, a bypass valve 207, a solenoid valve 208, a molecular pump 209, a gate valve 210, and two gas extraction pipes. The mechanical pump 206 and the molecular pump 209 are connected through one gas extraction pipe connected to the outside atmosphere. The molecular pump 209 and one gas extraction pipe of the gas control box are provided with the solenoid valve 208. The gate valve 210 is arranged on one gas extraction pipe between the mechanical pump 206 and the molecular pump 209. One end of the other gas extraction pipe is connected to one gas extraction pipe between the mechanical pump 206 and the gate valve 210. The other end of the other gas extraction pipe is connected to the outside atmosphere. The bypass valve 207 is arranged on the other gas extraction pipe. The gas extraction path is located in the gas control box.
[0061] The gas extraction passage is used to extract the gas in the vacuum chamber 101 to ensure the high pressure environment required in the experiment operation. Two different modes are adopted under different working conditions: high pressure and low pressure modes. When the atmosphere needs to be quickly extracted in the low pressure state, the mechanical pump 206 and the side extraction valve 207 can be opened, and the mechanical pump 206 can quickly and effectively extract the atmosphere into the equipment. When the internal pressure of the vacuum chamber reaches a certain pressure, the electromagnetic valve 208 and the mechanical pump 206 are opened, and the side extraction valve 207 is closed. At this time, the mechanical pump 206 and the side extraction valve 207 jointly complete the pretreatment and primary extraction of the gas. Then, the electromagnetic valve 208 starts to work to inject the gas into the molecular pump 209. In order to better protect the molecular pump 209, a gate valve 210 is arranged above the molecular pump 209 to balance the gas pressure and protect the molecular pump 209. Under the control of the side extraction valve 207 and the gate valve 210, the gas extraction passage can quickly and stably extract the gas to ensure that the gas pressure in the chamber is stably controlled below 4*10 -4 Pa to meet the requirements of normal operation of the equipment. The gas control box realizes firm support for the chamber 101 through a plurality of branch pipes.
[0062] The mechanical pump 206 and the side extraction valve 207 of the gas control module 20 are used to avoid the pollution of the vacuum chamber module by other gases and to preliminarily reduce the gas pressure in the chamber. The molecular pump 209, the electromagnetic valve 208 and the gate valve 209 are used to avoid the pollution of the vacuum chamber by other gases, to reduce the gas pressure in the chamber, and to further reduce the gas pressure to make the chamber reach a high vacuum degree. The gas exhaust valve 204 is used to put gas into the chamber after the evaporation is completed to balance the internal and external gas pressures.
[0063] The evaporation method of the peptide film evaporation equipment of the present application comprises the following steps:
[0064] Step one: two substrates are respectively pasted at the bottom center of the two sample holders 104 of the deposition area module 10 and face the circular through slot of the respective sample holder seat 105, and the target material is placed on the two evaporation pans 301 of the heating module 30. The substrate is glass, silicon wafer, metal or polymer substrate; the target material is made of peptide powder material, and the deposition amount of the target material is between 0.1 mg and 150.0 mg.
[0065] Step two: the output shaft of the stepping motor 119 of the lifting part of the rotary lifting device of the deposition area module 10 rotates in turn to drive the small pulley 120, the transmission belt 121, the large pulley 122 and the transmission screw 123 to rotate around their respective axes, drive the transmission nut 124 to move along the length direction of the transmission screw 123, thereby drive the corrugated tube upper flange 126 through the moving plate 125 to make the rotary part as a whole move along the length direction of the transmission screw 123 to drive the two sample holders of the evaporation deposition device as a whole through the fixed plate 135, until the pointer on the moving plate 125 points to the preset mark on the scale 132, so that the distance between each substrate and the corresponding target material is equal to the preset distance, and the stepping motor 119 is stopped. The distance between the target material and the substrate can be as small as 10 mm.
[0066] Step three: open the mechanical pump 206 and the bypass valve 207 of the gas control module 20, rapidly pump out the atmosphere through the mechanical pump 206, until the gas pressure in the gas control box reaches 20 Pa; close the bypass valve 207, open the electromagnetic valve 208, the molecular pump 209 and the shutter valve 210, and reduce the gas pressure in the chamber 101 to 4x10 -4 Pa through the molecular pump 209.
[0067] Step four: heat the heating wire 303, and at the same time, the output shaft of the rotation motor 116 of the rotary part of the rotary lifting device of the deposition area module 10 rotates in turn to drive the rotation main tooth 117, the sample from tooth 114 and the rotation gear 113 of the two sample holders to rotate around their own central axes, thereby driving the two sample holders to rotate around the central axes of the respective rotation gears 113. The target material is heated at 400℃ for 10 min through the heat radiation of the heating wire 303, and a thin film is formed on the bottom surface of the substrate by sublimation and deposition of the target material.
[0068] Step five: open the nitrogen cylinder 201, the pressure reducing valve 203 and the gas release valve 204 of the gas control module 20, control the nitrogen cylinder 201 to inject a preset flow of nitrogen into the chamber 101 through the flow meter 202, until the gas pressure in the chamber 101 is equal to the atmospheric pressure, and open the chamber 101 to take out the peptide thin film deposited on the bottom surface of the substrate.
[0069] The base of the present application can be lifted, and the distance between the target material and the base can be as small as 10 mm; the heating mode is to heat the target material by heating wire through heat radiation. The peptide film includes a base and a peptide molecule array thereon, the peptide molecule array is obtained by self-assembly of peptide molecules in the evaporation process, and the peptide molecules are composed of two or more amino acids and their modified groups. In specific implementation, the device includes a deposition area module 10, a gas control module 20 and a heating module 30. The deposition area module 10 is used to provide a thin film deposition environment, the gas control module 20 is used to control the gas pressure of the deposition area module, and the heating module 30 is used to heat the target material, control the heating gradient and the deposition time. The deposition area module 10 includes a vacuum chamber 101 for maintaining high vacuum degree and a sample holder for fixing the base. The gas control module 20 includes a gas inlet for inputting reaction gas, an adjusting valve for controlling the flow and pressure of the reaction gas, and a gas discharge port for discharging reaction products and waste gas. The heating module 30 includes a heating wire for heating the target material and a controller for controlling the current and temperature of the heating wire.
Claims
1. A peptide thin film evaporation equipment based on physical vapor deposition technology, characterized in that: It includes a deposition area module (10), a gas control module (20) and a heating module (30). The heating module (30) is installed inside the lower side of the deposition area module (10), and the gas control module (20) is connected to the interior of the deposition area module (10). The deposition area module (10) includes a rotary lifting device and a vapor deposition device. The rotary lifting device is installed on the top of the vapor deposition device, and the vapor deposition device is connected to the gas control module (20). The vapor deposition apparatus includes a vacuum chamber (101) and two sample holders. The bottom end of the rotary lifting device extends into the interior of the chamber (101) and is connected to the top surface of a horizontally arranged fixed plate (135). The two sample holders are symmetrically installed on the upper side of the interior of the chamber (101) through the fixed plate (135). The top of the two sample holders and the lower sides of the rotary lifting device are engaged. The heating module (30) is located directly below the two sample holders. The chamber (101) is connected to the gas control module (20) through a pipe (205). The sample holder includes a sample holder (104), a sample holder base (105), a conductive ring (106), a ceramic ring (107), a round cover (108), a large cylinder (109), a large bottom ring (110), a long cylinder (111), a small bottom ring (112), and a rotating gear (113). The sample holder base (105), conductive ring (106), ceramic ring (107), round cover (108), large cylinder (109), large bottom ring (110), long cylinder (111), small bottom ring (112), and rotating gear (113) are arranged horizontally and concentrically from bottom to top. The large cylinder (109) and large bottom ring (110) are respectively arranged on the fixed plate (13). 5) Bottom and top surfaces, the large bottom ring (110) is fitted on the outside of the long cylinder (111), the bottom end of the long cylinder (111) passes through the large bottom ring (110) and the fixing plate (135) and is connected to the top of the large cylinder (109); the side of the sample holder (105) is provided with an installation groove facing inward, and the sample holder (104) is concentrically arranged in the installation groove of the sample holder (105); the self-rotating gear (113) meshes with the lower part of the rotating lifting device; the bottom of the sample holder (105) is provided with a circular through groove that passes through the installation groove, the center of the bottom surface of the sample holder (104) is directly opposite the circular through groove, and the heating module (30) is located directly below the two circular through grooves; The rotary lifting device includes a rotating part and a lifting part. The lifting part includes a stepper motor (119), a small pulley (120), a conveyor belt (121), a large pulley (122), a transmission screw (123), a transmission nut (124), a moving connecting plate (125), a bellows upper flange (126), a bellows (127), a loose flange (128), a lower fixing plate (129), an upper fixing plate (130), a support guide shaft (131), a limit block (133), and a mounting plate. The upper end of the main shaft (134) is connected to the bottom end of the bellows (127). The bellows upper flange (126) is fitted on the upper end of the bellows (127). The loose flange (128) is fitted on the connection between the bellows (127) and the main shaft (134). The outer side of the loose flange (128) is connected to one side of the horizontally arranged lower fixing plate (129). The lifting part also includes a scale (132), which is vertically installed between the lower fixed plate (129) and the upper fixed plate (130) and close to the transmission screw (123). The moving connecting plate (125) has a horizontal pointer on the side of the scale (132) close to the scale, and the end of the pointer points to the scale (132). The heating module (30) includes two heaters, each heater including an evaporating dish (301), a boron nitride sheet (302), a heating wire (303), a heat-dissipating plate (304), two ceramic tubes (305), an upper heating shield (306), an inner heating shield (307), an outer heating shield (308), a heat insulation plate (309), and an outer heating shield (310). The heat-dissipating plate (304) is a stepped cylindrical hollow cylinder. The structure includes an inverted frustum groove inside the upper cylinder of the heat-uniform plate (304) and a cylindrical groove inside the lower cylinder of the heat-uniform plate (304). The outer diameter of the upper cylinder of the heat-uniform plate (304) is larger than that of the lower cylinder. The evaporating dish (301) is in the shape of an inverted frustum and is placed in the inverted frustum groove of the upper cylinder of the heat-uniform plate (304). The evaporating dish (301) is directly opposite to and located on the sample holder (105) of its respective sample holder. Directly below the circular through-slot, a boron nitride sheet (302) is horizontally installed in the cylindrical groove of the lower cylinder of the heat-dissipating plate (304). A heat insulation plate (309) is horizontally installed and covers the bottom end of the heat-dissipating plate (304). A heating wire (303) is spirally wound on the outer ring surface of the boron nitride sheet (302). Both ends of the heating wire (303) pass downward through the heat insulation plate (309), and both ends of the heating wire (303) are fitted with ceramic tubes (305). The outer side of the lower cylinder of the plate (304) is fitted with an inner heating shield (307) and an outer heating shield (308) in sequence. The upper end of the upper heating shield (306) is fitted on the outer side of the outer heating shield (308). The outer heating shield (310) is fitted on the outer side of the upper cylinder of the heat equalization plate (304) and the upper heating shield (306). The upper heating shield (306) is installed on the lower side of the interior of the chamber (101) by means of a mounting bracket.
2. The peptide thin film evaporation equipment based on physical vapor deposition technology according to claim 1, characterized in that: The rotating part includes a sample follower gear (114), a motor support plate (115), a self-rotating motor (116), a self-rotating main gear (117), and a main shaft (134). The main shaft (134) is arranged vertically, and its lower end is connected to the center of the top surface of the fixed plate (135). The sample follower gear (114) is fitted onto the lower part of the main shaft (134). A horizontal gear is provided at both the upper and lower ends of the sample follower gear (114), located outside and inside the chamber (101) respectively. The gear at the lower end of the sample follower gear (114) The rotating gears (113) of the two sample holders mesh with each other; the rotating motor (116) and the rotating main gear (117) are mounted on the outer top surface of the chamber (101) through the motor support plate (115). The rotating motor (116) is located directly above the rotating main gear (117). The rotating main gear (117) is arranged horizontally. The output shaft of the rotating motor (116) is synchronously connected to the center of the rotating main gear (117). The gear at the upper end of the sample tooth (114) is located on the motor support plate (115) and meshes with the rotating main gear (117). The bottom surface of the lower fixed plate (129) away from the main shaft (134) is connected to the top surface of one side of the horizontally arranged mounting plate. The stepper motor (119) is mounted on the top surface of the other side of the mounting plate. The output shaft of the stepper motor (119) passes vertically downward through the mounting plate and is synchronously connected to the center of the small pulley (120). The upper fixed plate (130) is horizontally mounted directly above the lower fixed plate (129) through a vertically arranged support guide shaft (131). The bottom end of the support guide shaft (131) passes through the lower fixed plate (129) and is connected to the top surface of the mounting plate. A vertically arranged transmission screw (123) is also installed between the lower fixed plate (129) and the upper fixed plate (130). The bottom end of the transmission screw (123) is attached to the top surface of the mounting plate. After passing through the lower fixed plate (129) and the mounting plate, it is synchronously connected to the center of the large pulley (122). The large pulley (122) and the small pulley (120) are at the same height. The small pulley (120) is connected to the large pulley (122) through the transmission belt (121). The transmission screw (123) is threaded with a transmission nut (124). The transmission nut (124) is connected to one side of the horizontally arranged movable connecting plate (125). The other side of the movable connecting plate (125) is supported on the bottom surface of the bellows flange (126). The transmission screw (123) and the support guide shaft (131) are also provided with a limit block (133). The limit block (133) is located between the transmission nut (124) and the lower fixed plate (129).
3. The peptide thin film evaporation equipment based on physical vapor deposition technology according to claim 2, characterized in that: The bellows (127) includes two bellows pipe fittings (127a), two bellows connectors (127b), and a bellows plate (127c). The two bellows pipe fittings (127a) are located on the upper and lower sides of the bellows plate (127c) and are arranged vertically and coaxially. The two ends of the bellows plate (127c) are connected to the two bellows pipe fittings (127a) through the two bellows connectors (127b). The expansion and contraction direction of the bellows plate (127c) is vertical. The upper flange (126) of the bellows is fitted on the upper end of the upper bellows pipe fitting (127a), and the lower end of the lower bellows pipe fitting (127a) is coaxially connected to the upper end of the main shaft (134). The loose flange (128) is fitted on the connection between the lower end of the lower bellows pipe fitting (127a) and the upper end of the main shaft (134).
4. The peptide thin film evaporation equipment based on physical vapor deposition technology according to claim 3, characterized in that: The gas control module (20) includes a gas control box, a venting passage and a pumping passage. The venting passage includes a nitrogen cylinder (201), a flow meter (202), a pressure reducing valve (203), a venting valve (204) and a venting pipe. The nitrogen cylinder (201) is connected to the chamber (101) of the deposition area module (10) through the venting pipe and the connecting pipe (205) in sequence. The pressure reducing valve (203) and the venting valve (204) are installed in sequence on the venting pipe between the nitrogen cylinder (201) and the connecting pipe (205). The flow meter (202) is installed on the venting pipe between the nitrogen cylinder (201) and the pressure reducing valve (203). The nitrogen cylinder (201), the flow meter (202) and the pressure reducing valve (203) are located outside the gas control box, and the venting valve (204) is located inside the gas control box. The gas extraction passage includes a mechanical pump (206), a bypass valve (207), a solenoid valve (208), a molecular pump (209), a gate valve (210), and two extraction pipes. The mechanical pump (206) and the molecular pump (209) are connected by an extraction pipe that connects to the outside atmosphere. A solenoid valve (208) is installed on one extraction pipe between the molecular pump (209) and the gas control box. A gate valve (210) is installed on one extraction pipe between the mechanical pump (206) and the molecular pump (209). One end of another extraction pipe is connected to one extraction pipe between the mechanical pump (206) and the gate valve (210). The other end of the other extraction pipe connects to the outside atmosphere. A bypass valve (207) is installed on the other extraction pipe. The gas extraction passage is located inside the gas control box.
5. The vapor deposition method of the peptide thin film vapor deposition equipment according to claim 4, characterized in that: The method includes the following steps: Step 1: Attach the two substrates to the center of the bottom surface of the two sample holders (104) of the deposition area module (10) respectively and face the circular through groove of their respective sample holders (105). Place the target material on the two evaporating dishes (301) of the heating module (30). Step 2: The output shaft of the stepper motor (119) of the lifting part of the rotating lifting device of the deposition area module (10) rotates in sequence, driving the small pulley (120), the conveyor belt (121), the large pulley (122) and the transmission screw (123) to rotate around their respective axes, driving the transmission nut (124) to move along the length direction of the transmission screw (123), thereby driving the bellows flange (126) through the moving connecting plate (125) so that the rotating part as a whole drives the two sample holders of the vapor deposition device to move along the length direction of the transmission screw (123) through the fixed plate (135) until the pointer on the moving connecting plate (125) points to the preset mark on the scale (132), so that the distance between each substrate and its corresponding target material is equal to the preset distance, and the stepper motor (119) stops. Step 3: Open the mechanical pump (206) and bypass valve (207) of the gas control module (20) to remove atmospheric pressure until the gas pressure in the gas control box reaches 20 Pa; close the bypass valve (207), and open the solenoid valve (208), molecular pump (209), and gate valve (210) to reduce the gas pressure in the chamber (101) to 4 × 10 Pa using the molecular pump (209). -4 Pa; Step 4: The heating wire (303) is heated, and at the same time, the output shaft of the self-rotating motor (116) of the rotating part of the rotating lifting device of the deposition area module (10) rotates in sequence, driving the self-rotating main gear (117), the sample slave gear (114) and the self-rotating gears (113) of the two sample holders to rotate around their own central axis, thereby driving the two sample holders to rotate around the central axis of their respective self-rotating gears (113). The target material is rotated and heated for 10 minutes at 400°C by the thermal radiation of the heating wire (303), and the target material sublimates and deposits on the bottom surface of the substrate to form a thin film. Step 5: Open the nitrogen cylinder (201), pressure reducing valve (203) and venting valve (204) of the gas control module (20), and control the nitrogen cylinder (201) to inject nitrogen into the chamber (101) at a preset flow rate through the flow meter (202) until the gas pressure in the chamber (101) is equal to the atmospheric pressure. Open the chamber (101) and take out the peptide film deposited on the bottom surface of the substrate.
6. The vapor deposition method of the peptide thin film vapor deposition equipment according to claim 5, characterized in that: The substrate is glass, silicon wafer, metal or polymer substrate; the target is made of peptide powder material and the deposition amount of the target is between 0.1 mg and 150.0 mg.
Citation Information
Patent Citations
Multifunctional three-target magnetron sputtering coating device
CN216891178U