A method for manufacturing a rotating target of a tellurium compound

Abstract

The application belongs to the field of sputtering target material preparation, and discloses a preparation method of a tellurium compound rotating target material. The method comprises the following steps: (1) loading tellurium compound powder into a mold, and sequentially performing cold pressing and vacuum heating reaction in a vacuum hot pressing furnace to obtain a tellurium compound ingot; (2) using a processing machine tool to perform hole digging processing on the tellurium compound ingot obtained in step (1) to obtain a rotating target material cylinder, and binding the rotating target material cylinder section by section on a back pipe, so that the tellurium compound rotating target material is obtained after cleaning and drying. The application adopts a vacuum hot pressing method, first presses out a material ingot, and then performs pollution-free processing according to the size, so that the processed material can be continuously utilized, the cost is greatly saved, and the production efficiency is high.

Description

Technical Field

[0001] This invention belongs to the field of sputtering target preparation and relates to a method for preparing a tellurium compound rotating target. Background Technology

[0002] Tellurides are a class of compounds formed by tellurium and other elements. Their chemical formula is usually M. x Te y (M represents other metallic elements), where x and y are usually integers. Tellurium compounds are similar in some respects to sulfides and selenides and are commonly found in minerals. Some common tellurium compounds include lead tellurium oxide (PbTe), bismuth tellurium (Bi₂Te₃), germanium tellurium (GeTe), zinc tellurium (ZnTe), and aluminum tellurium (Al₂Te₃). These compounds possess important electrical, thermal, optical, and magnetic properties, and are therefore widely used in electronics, materials science, thermoelectric materials, semiconductor devices, and solar energy.

[0003] Commonly used sputtering targets are categorized by shape into planar targets and rotating targets. The target shape affects the stability and film characteristics of magnetron sputtering, as well as the target utilization rate. Therefore, changing the target shape design can improve coating quality and production efficiency, while saving costs. During magnetron sputtering with planar targets, the varying intensity of the magnetic field results in a concentrated annular "racetrack" on the target surface, leading to low target utilization. In contrast, rotating targets rotate during sputtering, constantly changing the sputtering zone, almost eliminating the sputtering racetrack seen with planar targets. This significantly improves utilization and saves production costs.

[0004] Therefore, it is necessary to develop a method for preparing tellurium compound rotating targets. Summary of the Invention

[0005] In view of the above-mentioned problems in the prior art, the purpose of this invention is to provide a method for preparing tellurium compound rotating targets that is cost-effective and has high production efficiency.

[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0007] A method for preparing a tellurium compound rotating target includes the following steps:

[0008] (1) The tellurium compound powder is loaded into a mold and placed in a vacuum hot press furnace for sequential cold pressing and vacuum heating reaction to obtain tellurium compound ingots; specifically:

[0009] The cold pressing pressure is 20~30MPa;

[0010] The vacuum hot pressing reaction is as follows: heat to 350~400℃, hold for 30~45min, then heat to 0.5T~0.9T, hot pressing pressure is 60~100MPa, hold for 60~90min; where T is the melting point of the tellurium compound.

[0011] (2) Use a machine tool to hollow out the tellurium compound ingot obtained in step (1) to obtain a rotating target cylinder. Bind the rotating target cylinder section by section to the back tube, clean and dry it to obtain the tellurium compound rotating target.

[0012] Preferably, in step (1), the vacuum hot pressing reaction is as follows: the temperature is increased to 350-400℃ at 8-15℃ / min, held for 30-45min, and then increased to 0.5T-0.9T at 8-15℃ / min, the hot pressing pressure is adjusted to 60-100MPa, and the temperature and pressure are held for 60-90min; where T is the melting point of the tellurium compound.

[0013] Preferably, in step (1), the telluride powder is one of zinc telluride powder, cadmium telluride powder, and bismuth telluride powder.

[0014] Preferably, in step (1), tellurium compound powder of -100 mesh is used.

[0015] Preferably, in step (1), the cold pressing process lasts for 10 to 30 minutes.

[0016] Preferably, in step (1), after the vacuum hot pressing reaction is completed, the mixture is cooled to room temperature and removed from the furnace to obtain tellurium compound ingots.

[0017] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0018] (1) The present invention adopts a vacuum hot pressing method to first press out material ingots, and then process them without pollution according to their size. The processed materials can be reused, which greatly saves costs and has high production efficiency.

[0019] (2) The preparation method of the present invention is simple and can be prepared on a large scale in industrial applications.

[0020] (3) The tellurium compound rotating target prepared by the present invention has a high target relative density and target bonding rate. Detailed Implementation

[0021] To address the aforementioned problems in the existing technology, the present invention aims to provide a cost-effective and highly efficient method for preparing tellurium compound rotating targets, comprising the following steps:

[0022] (1) The tellurium compound powder is loaded into a mold and placed in a vacuum hot press furnace for sequential cold pressing and vacuum heating reaction to obtain tellurium compound ingots; specifically:

[0023] The cold pressing pressure is 20~30MPa;

[0024] The vacuum hot pressing reaction is as follows: heat to 350~400℃, hold for 30~45min, then heat to 0.5T~0.9T, hot pressing pressure is 60~100MPa, hold for 60~90min; where T is the melting point of the tellurium compound.

[0025] (2) Use a machine tool to hollow out the tellurium compound ingot obtained in step (1) to obtain a rotating target cylinder. Bind the rotating target cylinder section by section to the back tube, clean and dry it to obtain the tellurium compound rotating target.

[0026] Preferably, in step (1), the vacuum hot pressing reaction is as follows: the temperature is increased to 350-400℃ at 8-15℃ / min, held for 30-45min, then increased to 0.5T-0.9T at 8-15℃ / min, the hot pressing pressure is adjusted to 60-100MPa, and held for 60-90min; where T is the melting point of the tellurium compound. The present invention sets the holding temperature at 350-400℃, which allows for better venting and is beneficial for increasing the density of the target material. Furthermore, setting the hot pressing temperature to 0.5-0.9T allows for better high-temperature sintering.

[0027] Preferably, in step (1), the telluride powder is one of zinc telluride powder, cadmium telluride powder, and bismuth telluride powder.

[0028] Preferably, in step (1), tellurium compound powder of -100 mesh is used.

[0029] Preferably, in step (1), the cold pressing process lasts for 10 to 30 minutes.

[0030] Preferably, in step (1), after the vacuum hot pressing reaction is completed, the mixture is cooled to room temperature and removed from the furnace to obtain tellurium compound ingots.

[0031] To facilitate understanding of the present invention, the present invention will be described more fully and in detail below with reference to preferred embodiments, but the scope of protection of the present invention is not limited to the following specific embodiments.

[0032] Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by those skilled in the art. The technical terms used herein are for the purpose of describing particular embodiments only and are not intended to limit the scope of the invention.

[0033] Example 1

[0034] This embodiment discloses a method for preparing a zinc telluride rotating target, including the following steps:

[0035] (1) Take 100-mesh zinc telluride powder, put it into a mold, and then put it into a vacuum hot press furnace;

[0036] First, cold pressing is performed at a pressure of 30 MPa for 12 minutes.

[0037] Then, a vacuum was drawn, and heating was turned on. The temperature was increased to 350℃ at a rate of 15℃ / min, and held for 30 minutes. Then, the temperature was increased to 900℃, and held for 90 minutes at a pressure of 70 MPa.

[0038] After cooling to room temperature, zinc telluride ingots are obtained from the furnace.

[0039] (2) The zinc telluride ingot obtained in step (1) is processed into a rotating target cylinder of the corresponding size by hollowing out the hole on an air-cooled CNC machining tool. The rotating target cylinder is bound to the back tube section by section, cleaned and dried to obtain zinc telluride rotating target material.

[0040] Example 2

[0041] This embodiment discloses a method for preparing a cadmium telluride rotating target, including the following steps:

[0042] (1) Take cadmium telluride powder of -100 mesh, put it into a mold, and then put it into a vacuum hot press furnace;

[0043] First, cold pressing is performed at a pressure of 20 MPa for 8 minutes.

[0044] Then, a vacuum was drawn, and heating was turned on. The temperature was increased to 400℃ at 8℃ / min and held for 45min. Then, the temperature was increased to 800℃ and held for 70min at 100MPa.

[0045] After cooling to room temperature, cadmium telluride ingots are obtained from the furnace.

[0046] (2) The cadmium telluride ingot obtained in step (1) is machined into a rotating target cylinder of the corresponding size by hollowing out the hole on an air-cooled CNC machining tool. The rotating target cylinder is then bound to the back tube section by section, cleaned, and dried to obtain the cadmium telluride rotating target.

[0047] Example 3

[0048] This embodiment discloses a method for preparing a bismuth telluride rotating target, including the following steps:

[0049] (1) Take bismuth telluride powder of -100 mesh, put it into a mold, and then put it into a vacuum hot press furnace;

[0050] First, cold pressing is performed at a pressure of 25 MPa for 10 minutes.

[0051] Then, a vacuum was drawn, and heating was turned on. The temperature was increased to 400℃ at 10℃ / min and held for 45min. Then, the temperature was increased to 500℃ and held for 80min at 100MPa.

[0052] After cooling to room temperature, bismuth telluride ingots are obtained from the furnace.

[0053] (2) The bismuth telluride ingot obtained in step (1) is machined into a rotating target cylinder of the corresponding size by hollowing out the hole on an air-cooled CNC machining tool. The rotating target cylinder is then bound to the back tube section by section, cleaned, and dried to obtain the bismuth telluride rotating target.

[0054] Comparative Example 1

[0055] This comparative example discloses a method for preparing a bismuth telluride rotating target, comprising the following steps:

[0056] (1) Take 100-mesh zinc telluride powder, put it into a mold, and then put it into a vacuum hot press furnace;

[0057] First, cold pressing is performed at a pressure of 30 MPa for 12 minutes.

[0058] Then, a vacuum was drawn, and heating was turned on. The temperature was increased to 900℃ at a rate of 15℃ / min, and the temperature and pressure were maintained for 90min at a pressure of 70MPa.

[0059] After cooling to room temperature, zinc telluride ingots are obtained from the furnace.

[0060] (2) The zinc telluride ingot obtained in step (1) is processed into a rotating target cylinder of the corresponding size by hollowing out the hole on an air-cooled CNC machining tool. The rotating target cylinder is bound to the back tube section by section, cleaned and dried to obtain zinc telluride rotating target material.

[0061] Comparative Example 2

[0062] This comparative example discloses a method for preparing a bismuth telluride rotating target, comprising the following steps:

[0063] (1) Take 100-mesh zinc telluride powder, put it into a mold, and then put it into a vacuum hot press furnace;

[0064] First, cold pressing is performed at a pressure of 30 MPa for 12 minutes.

[0065] Then, a vacuum was drawn, and heating was turned on. The temperature was increased to 350℃ at a rate of 15℃ / min, and held for 30 minutes. Then, the temperature was increased to 550℃, and held for 90 minutes at 70 MPa.

[0066] After cooling to room temperature, zinc telluride ingots are obtained from the furnace.

[0067] (2) The zinc telluride ingot obtained in step (1) is processed into a rotating target cylinder of the corresponding size by hollowing out the hole on an air-cooled CNC machining tool. The rotating target cylinder is bound to the back tube section by section, cleaned and dried to obtain zinc telluride rotating target material.

[0068] The zinc telluride rotating targets obtained in Examples 1-3 and Comparative Example 1 / 2 were tested, and the test data are shown in Table 1.

[0069] Table 1

[0070] Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 relative density of target material 98.3% 98.7% 97.8% 95.6% 85% binding rate 99% 99.3% 99.3% 99.1% 99%

[0071] It can be seen that the tellurium compound rotating target prepared by the method of the present invention has a high target relative density and target bonding rate.

[0072] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of the present invention.

Claims

1. A method for preparing a tellurium compound rotating target, characterized in that, Includes the following steps: (1) The tellurium compound powder is loaded into a mold and placed in a vacuum hot press furnace for sequential cold pressing and vacuum heating reaction to obtain tellurium compound ingots; specifically: The telluride powder is one of zinc telluride powder, cadmium telluride powder, and bismuth telluride powder. The cold pressing pressure is 20~30MPa, and the cold pressing time is 10~30min; The vacuum hot pressing reaction is as follows: the temperature is increased to 350-400℃ at a rate of 8-15℃ / min, held for 30-45min, then increased to 0.5T-0.9T at a rate of 8-15℃ / min, the hot pressing pressure is adjusted to 60-100MPa, and the temperature and pressure are held for 60-90min; where T is the melting point of the tellurium compound. (2) Use a machine tool to hollow out the tellurium compound ingot obtained in step (1) to obtain a rotating target cylinder. Bind the rotating target cylinder section by section to the back tube, clean and dry it to obtain the tellurium compound rotating target.

2. The method for preparing the tellurium compound rotating target as described in claim 1, characterized in that, In step (1), tellurium compound powder of -100 mesh is used.

3. The method for preparing the tellurium compound rotating target as described in claim 1, characterized in that, In step (1), after the vacuum hot pressing reaction is completed, the mixture is cooled to room temperature and removed from the furnace to obtain tellurium compound ingots.