ErD x Preparation method and product
By optimizing the ErDx preparation process using magnetron sputtering technology, the problems of low preparation efficiency and the influence of oxide impurities in existing technologies have been solved, enabling the efficient preparation of ErDx thin films with high deuterium content and improving the nuclear reaction rate and stability.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-11
- Publication Date
- 2026-03-31
AI Technical Summary
Existing ErDx preparation methods are inefficient, unable to prepare compounds with high deuterium content, and suffer from the problem of oxide impurities affecting the nuclear reaction rate.
By employing magnetron sputtering technology and controlling the gas flow ratio and sputtering power supply current, the ErDx preparation process is optimized, including pre-sputtering cleaning and precise control of sputtering process parameters, to form ErDx thin films with high deuterium content.
This improved the preparation efficiency of ErDx, reduced the oxide content, enhanced the stability and adhesion of the film to the substrate, increased the yield of nuclear reactions, and simplified the preparation process.
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Figure CN118996355B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of materials preparation technology and relates to ErD. x Preparation, particularly relating to an ErD based on magnetron sputtering x Preparation method and product. Background Technology
[0002] Over the past few decades, erbium deuteride (ErD) x ErD2, as an important nuclear material, is widely used as a neutron generator target due to its strong hydrogen storage capacity and good thermal stability. In the diagnostic systems of inertial confinement fusion (ICF) devices such as NIF (National Ignition Facility), OMEGA, and Z, ErD2 is the most commonly used proton source target for proton diagnostic system calibration, for example, through… 3 He beam bombardment ErD x The target material generates calibration protons. Research has found that ErD... x Deuterium content, bulk oxidation, and thermal stability significantly influence nuclear reaction rates. Clearly, increasing and controlling ErD... x The D content is a relatively important process.
[0003] ErD2 thin film target preparation typically employs a two-step method, involving erbium film preparation and deuterium loading. In the first step, the erbium film is evaporated using an electron beam. To eliminate the problems of erbium film cracking and peeling, the evaporation rate is generally controlled to 10 nm / min. The second step, deuterium loading, mainly includes either non-air exposure loading or air exposure loading. Provo et al. published a history of very thick films and bulk samples of group IIIB, IVB, VB, and rare earth materials for various vacuum applications. They mentioned that producing a 50 μm deuterated erbium film required a total of 84 hours. This long time was necessary to obtain a film without peeling, but the complex process and the extended time spent at each step undoubtedly led to reduced production efficiency [see Provo, James L. History of very thick film and bulk sample group IIIB, IVB, VB, and rare earth materials for various vacuum applications. Journal of Vacuum Science & Technology A36.4 (2018)]. The problem with the two-step method is that the surface of the prepared erbium film contains oxides, making it difficult for deuterium atoms to enter the erbium film and form erbium deuteride, which greatly slows down the deuteration rate. Although the increased thermal activation process increases the reaction rate, it also leads to more oxygen entering the bulk, causing deuterium atoms in the Er lattice to be replaced by oxygen atoms, which undoubtedly reduces the nuclear reaction rate to a great extent.
[0004] Adams et al. investigated the microstructure, phase formation, and stress of reactively-deposited metal hydride films by ion sputtering. They used a Kaufmann ion source to sputter-deposit erbium hydride films in a hydrogen atmosphere. The problem was that there were almost no oxides in the erbium hydride bulk at deposition temperatures below 400 °C, while slightly more oxygen was found above 400 °C [see Adams, David P., et al. Microstructure, phase formation, and stress of reactively-deposited metalhydride thin films. No. SAND 2002-1466. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Sandia National Lab. (SNL-CA), Livermore, CA (United States), 2002]. Summary of the Invention
[0005] The purpose of this invention is to address the shortcomings of existing technologies in the preparation of ErD.x To address the issues of low efficiency and inability to prepare compounds with higher deuterium content, a magnetron sputtering-based ErD method is provided. x The preparation method can improve ErD x The preparation efficiency is improved, and high deuterium content is achieved by controlling the gas flow ratio and sputtering power supply current.
[0006] To achieve the above objectives, the present invention adopts the following technical solutions.
[0007] The present invention provides an ErD based on magnetron sputtering x The preparation method includes the following steps:
[0008] S1 evacuates the magnetron sputtering equipment to a vacuum level below 2 × 10⁻⁶. -3 Pa, then Ar gas is introduced;
[0009] S2 pre-sputters the erbium target under Ar gas conditions;
[0010] After S3 pre-sputtering, the total pressure of Ar and D2 gas is controlled at 0.3-1.0 Pa, and the flow ratio of D2 gas to Ar gas is 2:3-4:3.
[0011] S4 controls the sputtering power supply to sputter erbium onto the substrate using the ErD sputtering method. x Once the set thickness is reached, ErD is obtained. x Thin film; the sputtering power supply is a pulse power supply or an RF power supply; when the sputtering power supply is a pulse power supply, its current is controlled to be 100-500mA, the matching voltage is 300-550V, and the duty cycle is 30%-100%; when the sputtering power supply is an RF power supply, its power is controlled to be 150-300W.
[0012] In step S2 above, the baffle is closed, the Ar gas pressure is controlled at 0.3-1.0 Pa, and the erbium target is pre-sputtered and cleaned for 10-15 minutes. The sputtering power supply is a pulse power supply or an RF power supply. When the sputtering power supply is a pulse power supply, its current is controlled at 100-500mA, the matching voltage is controlled at 300-550V, and the duty cycle is controlled at 30%-100%. When the sputtering power supply is an RF power supply, its power is controlled at 150-300W.
[0013] In step S3 above, the total pressure of Ar gas and D2 gas is preferably 0.45-0.6 Pa.
[0014] In steps S2 or S4 above, when the sputtering power supply is a pulse power supply, the current is preferably 200-300mA, the matching voltage is 360-430V, the duty cycle is preferably 40-60%, and the sputtering time is controlled according to the thickness requirements; when the sputtering power supply is an RF power supply, the sputtering power is preferably 150-200W.
[0015] In step S4 above, the substrate can be Mo or Si; the distance between the erbium target and the substrate is 8-15 cm.
[0016] This invention also provides ErD prepared by the above method. x Thin film products; the ErD x In the thin film, x ranges from 2 to x ≤ 3; ErD x The film thickness can be precisely controlled by the deposition rate. The ErD film prepared by the method of this invention... x The film thickness is 3-5 μm. And the ErD... x The thin film has a very low oxygen content and a cubic crystal structure.
[0017] Compared with the prior art, the ErD based on magnetron sputtering provided by this invention x The preparation method and product have the following beneficial effects:
[0018] (1) Based on magnetron sputtering technology, this invention can increase the deuterium content in deuterides by controlling the gas flow rate and sputtering power supply control parameters, which is beneficial to increasing the nuclear reaction yield per unit time;
[0019] (2) This invention is based on magnetron sputtering technology. By controlling the gas flow rate and sputtering power supply control parameters, the oxygen content can be greatly reduced to form cubic ErD phase. x This effectively avoids unnecessary nuclear reaction spikes and deuterium atom diffusion barriers during TDS analysis;
[0020] (3) This invention is based on magnetron sputtering technology, and ErD is prepared by controlling the gas flow rate and sputtering power supply control parameters. x It has a high decomposition temperature, stable performance, and strong bonding force with the matrix, which can effectively resist the instability of target film decomposition and shedding caused by the temperature rise of nuclear reaction (or ion bombardment).
[0021] (4) This invention is based on magnetron sputtering technology, and ErD can be achieved by controlling the gas flow rate and sputtering power. x The preparation method greatly simplifies the preparation conditions, reduces the preparation time, and improves the preparation efficiency, making it suitable for widespread use in this field.
[0022] (5) This invention is based on magnetron sputtering technology, and the method of controlling the flow rate of D2 gas is applied to the prepared cubic ErD2. x XRD identification of thin films has unique effects, such as identifying ErD2 or ErD3 by the preferential deposition changes of close-packed surfaces in magnetron sputtering, which is superior to existing technologies. Attached Figure Description
[0023] Figure 1 The Mo-based ErD prepared in Example 1 of this inventionx Thin film photograph (a) and cubic ErD3 lattice structure (b); wherein Er atoms are arranged in a face-centered cubic framework, and D... O D represents a deuterium atom occupying an octahedral site. T The deuterium atom occupying a tetrahedral site is shown. For clarity and ease of understanding, the crystal plane in Figure (b) is labeled with equivalent planes.
[0024] Figure 2 The Mo-based ErD prepared in Examples 1-3 of this invention x Thin film XRD analysis results;
[0025] Figure 3 The silicon-based ErD prepared in Examples 1-3 of this invention x Thin film SEM analysis results; where (a) corresponds to a deuterium gas flow rate of 4 sccm, (b) corresponds to a deuterium gas flow rate of 6 sccm, and (c) corresponds to a deuterium gas flow rate of 8 sccm;
[0026] Figure 4 The Mo-based ErD prepared in Example 1 of this invention x Thin film EDS analysis results;
[0027] Figure 5 The Mo-based ErD prepared in Examples 1-3 of this invention x Thin film TDS analysis results; where (a) is the thermal desorption spectrum and (b) is the calculated statistical results of the low temperature peak (the proportion of D atoms occupying octahedral sites). Detailed Implementation
[0028] The technical solutions of various embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0029] Example 1
[0030] In this embodiment, Mo and Si are used as substrates, with a spacing of 10 cm between the substrate and the erbium target. The radius of the erbium target is 2.5 cm. A pulsed power supply is used for sputtering.
[0031] This embodiment provides an ErD based on magnetron sputtering. x The preparation method includes the following steps:
[0032] S1 evacuates the magnetron sputtering equipment to a vacuum level of 2×10⁻⁶. -3 Pa, then Ar gas is introduced.
[0033] With the S2 baffle closed, the erbium target is pre-sputtered and cleaned. The pre-sputtering conditions are: Ar gas pressure controlled at 0.45 Pa, pulse power supply current at 200 mA (matched voltage at 360 V), duty cycle at 50%, and cleaning time at 10 min.
[0034] After S3 pre-sputtering is completed, the baffle is opened, and the total pressure of Ar and D2 gas is controlled at 0.48 Pa, with the Ar gas flow rate at 6 sccm and the D2 gas flow rate at 4 sccm.
[0035] The S4 control pulse power supply was set to a current of 200mA (matched voltage of 360V) and a duty cycle of 50%. Erbium target sputtering was performed for 45 minutes, resulting in ErD deposits on Mo and Si substrates, respectively. x film.
[0036] After sputtering, the prepared ErD x The thin film samples were stored in a dry argon atmosphere to slow down the oxidation rate.
[0037] Example 2
[0038] In this embodiment, Mo and Si are used as substrates, with a spacing of 10 cm between the substrate and the erbium target. The radius of the erbium target is 2.5 cm. A pulsed power supply is used for sputtering.
[0039] This embodiment provides an ErD based on magnetron sputtering. x The preparation method includes the following steps:
[0040] S1 evacuates the vacuum of the magnetron sputtering equipment to 1.5 × 10⁻⁶. -3 Pa, then Ar gas is introduced.
[0041] With the S2 baffle closed, the erbium target is pre-sputtered and cleaned. The pre-sputtering conditions are: Ar gas pressure controlled at 0.45 Pa, pulse power supply current at 200 mA (matched voltage at 360 V), duty cycle at 50%, and cleaning time at 10 min.
[0042] After S3 pre-sputtering is completed, the baffle is opened, and the total pressure of Ar and D2 gas is controlled at 0.50 Pa, with Ar gas flow rate at 6 sccm and D2 gas flow rate at 6 sccm.
[0043] The S4 control pulse power supply was set to a current of 200mA (matched voltage of 360V) and a duty cycle of 50%. Erbium target sputtering was performed for 45 minutes, resulting in ErD deposits on Mo and Si substrates, respectively. x film.
[0044] After sputtering, the prepared ErD x The thin film samples were stored in a dry argon atmosphere to slow down the oxidation rate.
[0045] Example 3
[0046] In this embodiment, Mo and Si are used as substrates, with a distance of 10 cm between the substrate and the erbium target. The radius of the erbium target is 2.5 cm. A pulsed power supply is used.
[0047] This embodiment provides an ErD based on magnetron sputtering. x The preparation method includes the following steps:
[0048] S1 evacuates the magnetron sputtering equipment to a vacuum level of 9×10⁻⁶. -4 Pa, then Ar gas is introduced.
[0049] With the S2 baffle closed, the erbium target is pre-sputtered and cleaned. The pre-sputtering conditions are: Ar gas pressure controlled at 0.45 Pa, pulse power supply current at 200 mA (matched voltage at 360 V), duty cycle at 50%, and cleaning time at 10 min.
[0050] After S3 pre-sputtering is completed, the baffle is opened, and the total pressure of Ar and D2 gas is controlled at 0.51 Pa, with the Ar gas flow rate at 6 sccm and the D2 gas flow rate at 8 sccm.
[0051] The S4 control pulse power supply was set to a current of 200mA (matched voltage of 360V) and a duty cycle of 50%. Erbium target sputtering was performed for 45 minutes, resulting in ErD deposits on Mo and Si substrates, respectively. x film.
[0052] After sputtering, the prepared ErD x The thin film samples were stored in a dry argon atmosphere to slow down the oxidation rate.
[0053] Example 4
[0054] In this embodiment, Mo and Si are used as substrates, with a spacing of 10 cm between the substrate and the erbium target. The radius of the erbium target is 2.5 cm. A pulsed power supply is used for sputtering.
[0055] This embodiment provides an ErD based on magnetron sputtering. x The preparation method includes the following steps:
[0056] S1 evacuates the magnetron sputtering equipment to a vacuum level of 1×10⁻⁶. -3 Pa, then Ar gas is introduced.
[0057] With the S2 baffle closed, the erbium target is pre-sputtered and cleaned. The pre-sputtering conditions are: Ar gas pressure controlled at 1 Pa, pulse power supply current at 100 mA (matched voltage at 300 V), duty cycle at 60%, and cleaning time at 10 min.
[0058] After S3 pre-sputtering is completed, the baffle is opened, and the total pressure of Ar and D2 gas is controlled at 0.47 Pa, with the Ar gas flow rate at 6 sccm and the D2 gas flow rate at 8 sccm.
[0059] The S4 control pulse power supply was set to 100mA (matched voltage 300V) with a duty cycle of 60%. Erbium target sputtering was performed for 60 minutes, resulting in ErD deposits on Mo and Si substrates, respectively. x film.
[0060] After sputtering, the prepared ErD x The thin film samples were stored in a dry argon atmosphere to slow down the oxidation rate.
[0061] Example 5
[0062] In this embodiment, Mo and Si are used as substrates, with a distance of 15 cm between the substrate and the erbium target. The radius of the erbium target is 2.5 cm. A pulsed power supply is used.
[0063] This embodiment provides an ErD based on magnetron sputtering. x The preparation method includes the following steps:
[0064] S1 evacuates the magnetron sputtering equipment to a vacuum level of 1×10⁻⁶. -3 Pa condition, then Ar gas is introduced.
[0065] With the S2 baffle closed, the erbium target is pre-sputtered and cleaned. The pre-sputtering conditions are: Ar gas pressure controlled at 1 Pa, pulse power supply current at 500 mA (matched voltage at 550 V), duty cycle at 100%, and cleaning time at 10 min.
[0066] After S3 pre-sputtering is completed, the baffle is opened, and the total pressure of Ar and D2 gas is controlled at 1 Pa, with Ar gas flow rate at 8 sccm and D2 gas flow rate at 8 sccm.
[0067] The S4 control pulse power supply has a current of 500mA (matched voltage of 550V) and a duty cycle of 100%. This 100% duty cycle means the pulse power supply is used as a DC power source. After sputtering an erbium target for 30 minutes, ErD values were obtained deposited on Mo and Si substrates, respectively. x Thin film. This implies a method for preparing a DC power source.
[0068] After sputtering, the prepared ErD x The thin film samples were stored in a dry argon atmosphere to slow down the oxidation rate.
[0069] Example 6
[0070] In this embodiment, Mo and Si are used as substrates, with a distance of 10 cm between the substrate and the erbium target. The radius of the erbium target is 2.5 cm. A pulsed power supply is used.
[0071] This embodiment provides an ErD based on magnetron sputtering. x The preparation method includes the following steps:
[0072] S1 evacuates the magnetron sputtering equipment to a vacuum level of 1×10⁻⁶. -3 Pa condition, then Ar gas is introduced.
[0073] With the S2 baffle closed, the erbium target is pre-sputtered and cleaned. The pre-sputtering conditions are: Ar gas pressure controlled at 0.3 Pa, pulse power supply current at 300 mA (matched voltage at 430 V), duty cycle at 40%, and cleaning time at 10 min.
[0074] After S3 pre-sputtering is completed, the baffle is opened, and the total pressure of Ar and D2 gas is controlled at 0.45 Pa, with Ar gas flow rate at 6 sccm and D2 gas flow rate at 6 sccm.
[0075] The S4 control pulse power supply was set to a current of 300mA (matched voltage of 430V) and a duty cycle of 40%. Erbium target sputtering was performed for 30 minutes to obtain ErD values deposited on Mo and Si substrates, respectively. x film.
[0076] After sputtering, the prepared ErD x The thin film samples were stored in a dry argon atmosphere to slow down the oxidation rate.
[0077] Example 7
[0078] In this embodiment, Si is used as the substrate, and the distance between the Si substrate and the erbium target is 8 cm. The radius of the erbium target is 2.5 cm. The sputtering power supply used is an radio frequency power supply.
[0079] This embodiment provides an ErD based on magnetron sputtering. x The preparation method includes the following steps:
[0080] S1 evacuates the magnetron sputtering equipment to a vacuum level of 2×10⁻⁶. -4 Pa, then Ar gas is introduced.
[0081] With the S2 baffle closed, the erbium target is pre-sputtered and cleaned. The pre-sputtering conditions are: Ar gas pressure controlled at 0.3 Pa, RF power supply power at 150 W, and cleaning time at 15 min.
[0082] After S3 pre-sputtering is completed, the baffle is opened, and the total pressure of Ar and D2 gas is controlled at 0.3 Pa, with the flow rate of D2 gas at 5 sccm and the flow rate of Ar gas at 5 sccm.
[0083] The S4 control RF power supply was set to 150W, and erbium target sputtering was performed for 60 minutes to obtain ErD deposited on the Si substrate. x film.
[0084] After sputtering, the prepared ErD x The thin film samples were stored in a dry argon atmosphere to slow down the oxidation rate.
[0085] Example 8
[0086] In this embodiment, Mo is used as the substrate, and the distance between the Mo substrate and the erbium target is 10 cm. The radius of the erbium target is 2.5 cm. An radio frequency power supply is used.
[0087] This embodiment provides an ErD based on magnetron sputtering. x The preparation method includes the following steps:
[0088] S1 evacuates the magnetron sputtering equipment to a vacuum level of 2×10⁻⁶. -4 Pa, then Ar gas is introduced.
[0089] With the S2 baffle closed, the erbium target is pre-sputtered and cleaned. The pre-sputtering conditions are: Ar gas pressure controlled at 0.45 Pa, RF power supply power at 300 W, and cleaning time at 15 min.
[0090] After S3 pre-sputtering is completed, the baffle is opened, and the total pressure of Ar and D2 gas is controlled at 0.5 Pa, the Ar gas flow rate is 6 sccm, and the D2 gas flow rate is 8 sccm.
[0091] The S4 control RF power supply was set to 300W, and erbium target sputtering was performed for 60 minutes to obtain ErD deposited on the Mo substrate. x film.
[0092] After sputtering, the prepared ErD x The thin film samples were stored in a dry argon atmosphere to slow down the oxidation rate.
[0093] The ErD prepared in Examples 1-3 above will be discussed below. x The thin film was subjected to structural and compositional analysis.
[0094] (I) Sample photographs and crystal structure
[0095] Mo-based ErD prepared in Example 1 x Photographs of thin film samples as follows Figure 1 (a) ErD3 crystal structure as shown in Figure 1 (b) where Er atoms are arranged in a face-centered cubic framework, D O D represents a deuterium atom occupying an octahedral site. TThis represents a deuterium atom occupying a tetrahedral position.
[0096] from Figure 1 (a) It can be seen that the prepared ErD x The film is blue and has a uniform and smooth morphology. From Figure 1 (b) It can be seen that in the face-centered cubic framework composed of Er atoms, ErD3 contains all octahedral and tetrahedral sites, while ErD2 mainly contains tetrahedral sites. Furthermore, all D atoms fill the equivalent (110) and (220) planes, while the atoms in the (111) plane remain unchanged when transitioning from ErD2 to ErD3. This characteristic significantly affects the close-packed preferential deposition of magnetron sputtering, and therefore ErD2 and ErD3 can be roughly distinguished by XRD testing.
[0097] (II) XRD Analysis
[0098] ErD prepared in Examples 1-3 x XRD analysis of the thin film was performed, and the results are as follows: Figure 2 As shown.
[0099] from Figure 2 It can be seen that when the D2 gas flow rate is 4 sccm, the hexagonal Er crystal planes in the film disappear, and the (111) plane maintains a certain height because its atomic density is not much different from that of (220). This means that all the sputtered Er atoms are converted into ErD2 under the deuterium atmosphere. When the D2 gas flow rate is 6 sccm and 8 sccm, with the continued increase of D in the (220) plane, the close-packed plane (220) becomes the preferred deposition direction for magnetron sputtering, causing the (111) peak to decrease rapidly and disappear when ErD3 is formed. Thus, the formation of ErD2 and ErD3 can be roughly determined.
[0100] (III) SEM Analysis
[0101] The Si-based ErD prepared in Examples 1-3 x The thin film was analyzed by SEM, and the results are as follows: Figure 3 As shown.
[0102] from Figure 3 It can be seen that the ErD prepared at deuterium gas flow rates of 4 sccm, 6 sccm, and 8 sccm... x The film thickness is approximately 3.7-4.2 μm; the film consists of a columnar crystal structure typical of magnetron sputtering.
[0103] (iv) EDS Analysis
[0104] Figure 4 For typical surface EDS elemental analysis, the ErD prepared in Examples 1-3 xThe oxygen atom percentages in the thin film samples were 6.01%, 3.38%, and 3.90%, respectively. Note that EDS cannot detect D atoms, therefore the total atomic count does not include D atoms when calculating the atomic ratio. Considering that the characterization was not performed in situ, the oxygen in the thin film samples may have originated from oxidation due to air exposure or from differences between different samples. However, this is a very low oxidation level compared to existing techniques (Er thermal diffusion deuteration techniques).
[0105] (V) Thermal Desorption TDS Analysis Results
[0106] Figure 5 (a) shows the thermal desorption spectra of the three samples. As can be seen from the figure, the low-temperature peak Peak1 is distributed in the range of 400-450℃, while the high-temperature peak Peak2 is concentrated around 790℃. Ion current signals and ErD can be calibrated using a standard leak and measured. x The atomic ratio of D to Er was calculated using the film thickness. The results show that ErD prepared at deuterium gas flow rates of 4 sccm, 6 sccm, and 8 sccm... x The D / Er atomic ratios of the thin films were 2:1, 2.5:1, and 3:1, respectively, and the peak area ratios of the low-temperature and high-temperature peaks basically conformed to the standard octahedral and tetrahedral occupancy ratios. These results are consistent with XRD analysis and reveal for the first time the occupancy problem of deuterium atoms in cubic erbium deuteride sputtered under uncontrolled temperature conditions.
[0107] In summary, the ErD developed in this invention x The thin film has high overall quality and the preparation method is convenient and effective, which is of great significance for accelerator target materials.
[0108] Those skilled in the art will recognize that the embodiments described herein are intended to help the reader understand the principles of the invention and should be understood as not limiting the scope of protection of the invention to such specific statements and embodiments. Those skilled in the art can make various other specific modifications and combinations based on the technical teachings disclosed in this invention without departing from the spirit of the invention, such as appropriately adjusting the sputtering current or power according to the size of the Er target used, or adjusting pre-sputtering conditions that do not affect the deposition process, etc., and these modifications and combinations are still within the scope of protection of this invention.
Claims
1. A magnetron sputter based ErD x Preparation method characterized in that, The method comprises the following steps: S1 The base vacuum of the magnetron sputtering equipment is pumped to below 2 x 10 -3 Pa condition, and then Ar gas is introduced; S2, pre-sputtering the erbium target under Ar gas; S3, after the pre-sputtering, controlling the total gas pressure of Ar gas and D2 gas to be 0.45-0.6 Pa, and the flow ratio of D2 gas to Ar gas to be 2:3-4:3; S4 controlling the sputtering power to sputter the erbium target to the substrate to form an ErD x to a set thickness to obtain the ErD x thin film; the sputtering power is a pulse power; when the sputtering power is a pulse power, the current is controlled to be 100-500 mA, the matching voltage is controlled to be 300-550 V, and the duty cycle is controlled to be 30%-100%.
2. The magnetron sputter-based ErD x Preparation method characterized in that, In step S2, the erbium target is pre-sputtered for cleaning, and the cleaning time is 10-15 min; the sputtering power source is a pulse power source, and the current is controlled to be 100-500 mA, the matching voltage is controlled to be 300-550 V, and the duty cycle is controlled to be 30%-100%.
3. The magnetron sputter-based ErD x Preparation method characterized in that, The current of the pulse power source is 200-300 mA, the matching voltage is 360-430 V, and the duty cycle is 40-60%.
4. A magnetron sputter based ErD x Preparation method characterized in that, The substrate is Mo or Si; and the distance between the erbium target and the substrate is 8-15 cm.
5. ErD prepared by the method of any one of claims 1 to 4 x Thin film product.
6. The ErD of claim 5 x A thin film product characterized by The ErD x x in the thin film ranges from 2 to 3.
7. The ErD of claim 5 x A thin film product characterized by ErD x The film thickness is 3-5 μm.
Citation Information
Patent Citations
Preparation method for deuterium-containing metal film target
CN106544628A