Ytterbium oxide doped indium scandium oxide crystal film and preparation method thereof
By adding ytterbium oxide and scandium oxide to the indium oxide matrix, adjusting the doping amount, and deposition of ytterbium oxide-doped indium oxide crystal thin film by magnetron sputtering method, the high resistivity of oxide targets in the prior art was solved. Problem, low resistivity and high carrier concentration crystal films are achieved, suitable for high-end display panels.
Patent Information
- Application Number
- CN202411295102.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-15
- Publication Date
- 2024-12-20
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
It is difficult to prepare low-resistivity crystal films with ytterbium oxide doped indium scandium oxide, and the electrical and optical properties of oxide targets are insufficient in high-end display panel applications.
By adding ytterbium oxide and scandium oxide to the indium oxide-based material, the doping amount of ytterbium and scandium is adjusted to increase carrier concentration and Hall mobility, thereby reducing the resistivity of the crystal film. Magnetically controlled sputtering is used The crystal film doped with ytterbium oxide is deposited with indium scandium oxide.
A low resistivity ytterbium oxide doped indium oxide crystal film is achieved, which improves carrier concentration and Hall mobility, and meets the performance requirements of high-end display panels.
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Abstract
Description
Technical Field
[0001] The present application relates to the technical field of target material preparation, and in particular to a crystalline film of ytterbium oxide doped with indium scandium oxide and a preparation method thereof. Background Art
[0002] With the increasing market competitiveness of China's new display industry in recent years, as the world's largest TFT-LCD display panel production base, oxide targets have also become a research hotspot in China. Thin films sputtered using targets such as ZnO, IZO, and IGZO can be used for TFT active layers. In the application of LCD, OLED and electronic paper flat panel displays (FPD), they have attracted great attention from a large number of researchers and industry professionals due to their excellent performance.
[0003] The density, grain size, composition and structural uniformity of oxide targets affect various electrical and optical properties of sputtered films. In order to improve the quality of oxide targets to meet the needs of the high-end display panel industry, many researchers have improved and upgraded the powder raw materials of oxide targets.
[0004] Chinese patent application 202211636891.0 discloses an oxide target material and a preparation method thereof. The oxide target material includes an oxide of element A, an oxide of element B, an oxide of element R and an oxide of element M; element A is indium; element B is one or a combination of two or more of gallium, zinc and tin; element R is one or a combination of two or more of cerium, praseodymium, ytterbium, dysprosium and terbium; element M is one or a combination of two or more of scandium, silicon, titanium, tantalum, germanium and antimony.
[0005] This scheme refines the grain size of the oxide target by introducing the oxide of M into the oxide target, making the oxide target high in density and uniform in element distribution and microstructure;
[0006] Further observation of the scheme shows that the scheme does not attempt to sputter-coat the above-mentioned oxide target material and test the performance of the film.
[0007] The Chinese patent application discloses a high-mobility transparent conductive oxide film and a preparation method thereof. The TCO film is grown by reactive radio frequency magnetron sputtering to grow tellurium- and scandium-co-doped indium oxide TCO film at room temperature. The sputtering targets are indium target, tellurium target and scandium target, the sputtering working gas is argon, and the reaction gas is oxygen. Before the TCO film grows, only argon is introduced into the sputtering chamber, and the three targets are pre-sputtered for 15 to 30 minutes to remove impurities adsorbed on the surface of the target and surface oxides. When the TCO film starts to grow, argon and oxygen are fully mixed in the mixing chamber and then enter the sputtering chamber. The flow ratio of argon to oxygen is 50:1 to 20:1, and the sputtering pressure is 0.1 to 0.4 Pa. The sputtering power of the indium target is 200 W, the sputtering power of the tellurium target is 20 to 30 W, and the sputtering power of the scandium target is 1 to 2 W. The substrate deposition temperature is room temperature, and the sputtering time is 10 to 20 minutes.
[0008] This scheme produced a thin film with high carrier mobility, low resistivity and high light transmittance. However, observation of this scheme shows that, on the one hand, this scheme uses three targets for sputtering, and on the other hand, in this scheme, the distance between the target and the sample is 12 to 15 cm.
[0009] The problem that this proposal needs to solve is: how to propose a low-resistivity ytterbium oxide-doped indium scandium oxide crystalline film. Summary of the invention
[0010] The purpose of the present invention is to provide a low-resistivity ytterbium oxide-doped indium-scandium oxide crystal film. The scheme is to add ytterbium oxide, scandium oxide and other substances into a material based on indium oxide, thereby improving the Hall mobility and carrier concentration of the prepared crystal film and thus reducing the resistivity of the crystal film.
[0011] To achieve the above object, the present application discloses a crystalline film of ytterbium oxide doped with indium scandium oxide. The chemical formula of the crystalline film of ytterbium oxide doped with indium scandium oxide is In x Sc y Yb z O 3 , where 0.002≤y≤0.06, 0.001≤z≤0.03, and x+y+z=2.
[0012] The present application partially dopes ytterbium and scandium into an indium oxide-based material, and limits the doping amounts of ytterbium and scandium to increase the carrier concentration and Hall mobility of the crystal film, thereby suppressing the resistivity.
[0013] Preferably, the chemical formula of the ytterbium oxide doped indium scandium oxide crystal film is In x Sc y Yb z O 3, where 0.01≤y≤0.05, 0.01≤z≤0.025, and x+y+z=2.
[0014] Furthermore, during the experiment, we found that with the increase of doping elements, the carrier concentration of the crystal film does tend to increase, but the Hall mobility of the film will show a certain downward trend. Therefore, the doping amount of the doping element is further optimized to maintain a certain balance between the carrier concentration and the Hall mobility, so that the resistivity can be more fully reduced.
[0015] Preferably, the chemical formula of the ytterbium oxide doped indium scandium oxide crystal film is In x Sc y Yb z O 3 , where y=0.04, z=0.02, and x+y+z=2.
[0016] In addition, the present application also discloses a method for preparing the above-mentioned ytterbium oxide doped indium scandium oxide crystal film, comprising the following steps:
[0017] Step 1: Mixing, pressing and sintering ytterbium oxide powder, indium oxide powder and scandium oxide powder to obtain a target material of ytterbium oxide doped with indium oxide and scandium oxide;
[0018] Step 2: Deposit the ytterbium oxide doped indium scandium oxide target material obtained in step 1 onto an external substrate to obtain a crystalline film of ytterbium oxide doped indium scandium oxide.
[0019] Preferably, step 1 includes the following sub-steps:
[0020] Step A1: mixing ytterbium oxide powder, indium oxide powder and scandium oxide powder, then adding a binder, wet grinding and spray granulation to obtain a mixed powder;
[0021] Step A2: Pressing the mixed powder into a shape, and then sintering it to obtain a target material of ytterbium oxide doped with indium scandium oxide.
[0022] Preferably, in step 2, the deposition method for depositing the ytterbium oxide-doped indium scandium oxide target onto the substrate of the external device is magnetron sputtering.
[0023] Preferably, step 2 includes the following sub-steps:
[0024] Step B1: fixing a target material of ytterbium oxide doped with indium scandium oxide into a target holder of a magnetron sputtering deposition device;
[0025] Step B2: Turn on the radio frequency power supply to pre-deposit and clean the target material of ytterbium oxide doped indium scandium oxide;
[0026] Step B3: Then, the substrate is fixed on the sample stage, placed in the sputtering chamber, and the substrate is heated to 50-100° C. in a vacuum environment;
[0027] Step B4: Turn on the radio frequency power supply again to grow the crystalline film of ytterbium oxide doped with indium scandium oxide on the substrate to a thickness of 100±10 nm, thereby obtaining the crystalline film of ytterbium oxide doped with indium scandium oxide.
[0028] Preferably, in step B3, the distance between the ytterbium oxide doped indium scandium oxide target and the substrate is 6-8 cm.
[0029] The beneficial effects of the present invention are:
[0030] The present invention provides a low-resistivity ytterbium oxide-doped indium-scandium oxide crystal film, which reduces the resistivity of the crystal film by increasing the Hall mobility and carrier concentration of the prepared crystal film through doping ytterbium oxide, scandium oxide and other substances into a material based on indium oxide. DETAILED DESCRIPTION
[0031] In the description of the present invention, it should be noted that, if the specific conditions are not specified in the examples, the experiments were carried out according to conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used, if the manufacturer is not specified, are all conventional products that can be purchased commercially.
[0032] Example 1
[0033] Step 1:
[0034] Step A1: ytterbium oxide powder, indium oxide powder and scandium oxide powder are mixed at a molar ratio of indium, scandium and ytterbium of 1.992:0.004:0.004, and then a binder is added, and wet grinding and spray granulation are performed to obtain a mixed powder;
[0035] Step A2: Pressing the mixed powder into a shape, and then sintering it to obtain a target material of ytterbium oxide doped with indium scandium oxide.
[0036] Step 2:
[0037] Step B1: fixing a target material of ytterbium oxide doped with indium scandium oxide into a target holder of a magnetron sputtering deposition device;
[0038] Step B2: Turn on the RF power supply (sputtering power is 120W) to pre-deposit and clean the target of ytterbium oxide doped with indium scandium oxide;
[0039] Step B3: After cleaning, the quartz substrate is fixed on the sample stage, placed in the sputtering chamber and fixed so that the distance between the ytterbium oxide-doped indium scandium oxide target and the quartz substrate is 7 cm;
[0040] The vacuum degree of the growth chamber was evacuated to 3.3×10-3 Pa, the substrate is heated to 8°C, pure argon gas with a purity of more than 99.99% is introduced, and the pressure is controlled at 0.5Pa;
[0041] Step B4: Turn on the RF power supply again to grow the ytterbium oxide doped indium scandium oxide crystal film on the substrate to a thickness of 100±10nm, and obtain the ytterbium oxide doped indium scandium oxide crystal film. 1.992 Sc 0.004 Yb 0.004 O 3 The resistivity of the crystal film is 3.03×10 -4 Ω.cm, Hall mobility is 82.64cm 2 / Vs, the carrier concentration is 3.36×10 20 cm -3 .
[0042] Example 2
[0043] Step 1:
[0044] Step A1: mixing ytterbium oxide powder, indium oxide powder and scandium oxide powder according to a molar ratio of indium, scandium and ytterbium of 1.974:0.01:0.016, then adding a binder, wet grinding and spray granulation to obtain a mixed powder;
[0045] Step A2: Pressing the mixed powder into a shape, and then sintering it to obtain a target material of ytterbium oxide doped with indium scandium oxide.
[0046] Step 2:
[0047] Step B1: fixing a target material of ytterbium oxide doped with indium scandium oxide into a target holder of a magnetron sputtering deposition device;
[0048] Step B2: Turn on the RF power supply (sputtering power is 120W) to pre-deposit and clean the target of ytterbium oxide doped with indium scandium oxide;
[0049] Step B3: After cleaning, the quartz substrate is fixed on the sample stage, placed in the sputtering chamber and fixed so that the distance between the ytterbium oxide-doped indium scandium oxide target and the quartz substrate is 7 cm;
[0050] The vacuum degree of the growth chamber was evacuated to 3.3×10 -3 Pa, the substrate is heated to 80°C, pure argon gas with a purity of more than 99.99% is introduced, and the pressure is controlled at 0.5Pa;
[0051] Step B4: Turn on the RF power supply again to grow the ytterbium oxide doped indium scandium oxide crystal film on the substrate to a thickness of 100±10nm, and obtain the ytterbium oxide doped indium scandium oxide crystal film. 1.974 Sc 0.01Yb 0.016 O 3 The resistivity of the crystal film is 2.97×10 -4 Ω.cm, Hall mobility is 81.89cm 2 / Vs, the carrier concentration is 3.90×10 20 cm -3 .
[0052] Example 3
[0053] Step 1:
[0054] Step A1: ytterbium oxide powder, indium oxide powder and scandium oxide powder are mixed in a molar ratio of indium, scandium and ytterbium of 1.972:0.016:0.012, and then a binder is added, and wet grinding and spray granulation are performed to obtain a mixed powder;
[0055] Step A2: Pressing the mixed powder into a shape, and then sintering it to obtain a target material of ytterbium oxide doped with indium scandium oxide.
[0056] Step 2:
[0057] Step B1: fixing a target material of ytterbium oxide doped with indium scandium oxide into a target holder of a magnetron sputtering deposition device;
[0058] Step B2: Turn on the RF power supply (sputtering power is 120W) to pre-deposit and clean the target of ytterbium oxide doped with indium scandium oxide;
[0059] Step B3: After cleaning, the quartz substrate is fixed on the sample stage, placed in the sputtering chamber and fixed so that the distance between the ytterbium oxide-doped indium scandium oxide target and the quartz substrate is 7 cm;
[0060] The vacuum degree of the growth chamber was evacuated to 3.3×10 -3 Pa, the substrate is heated to 80°C, pure argon gas with a purity of more than 99.99% is introduced, and the pressure is controlled at 0.5Pa;
[0061] Step B4: Turn on the RF power supply again to grow the ytterbium oxide doped indium scandium oxide crystal film on the substrate to a thickness of 100±10nm, and obtain the ytterbium oxide doped indium scandium oxide crystal film. 1.972 Sc 0.016 Yb 0.012 O 3 The resistivity of the crystal film is 2.93×10 -4 Ω.cm, Hall mobility is 81.85cm 2 / Vs, the carrier concentration is 3.91×10 20 cm -3 .
[0062] Example 4
[0063] Step 1:
[0064] Step A1: ytterbium oxide powder, indium oxide powder and scandium oxide powder are mixed in a molar ratio of indium, scandium and ytterbium of 1.94:0.04:0.02, and then a binder is added, wet-grinded and spray-granulated to obtain a mixed powder;
[0065] Step A2: Pressing the mixed powder into a shape, and then sintering it to obtain a target material of ytterbium oxide doped with indium scandium oxide.
[0066] Step 2:
[0067] Step B1: fixing a target material of ytterbium oxide doped with indium scandium oxide into a target holder of a magnetron sputtering deposition device;
[0068] Step B2: Turn on the RF power supply (sputtering power is 120W) to pre-deposit and clean the target of ytterbium oxide doped with indium scandium oxide;
[0069] Step B3: After cleaning, the quartz substrate is fixed on the sample stage, placed in the sputtering chamber and fixed so that the distance between the ytterbium oxide-doped indium scandium oxide target and the quartz substrate is 7 cm;
[0070] The vacuum degree of the growth chamber was evacuated to 3.3×10 -3 Pa, the substrate is heated to 80°C, pure argon gas with a purity of more than 99.99% is introduced, and the pressure is controlled at 0.5Pa;
[0071] Step B4: Turn on the RF power supply again to grow the ytterbium oxide doped indium scandium oxide crystal film on the substrate to a thickness of 100±10nm, and obtain the ytterbium oxide doped indium scandium oxide crystal film. 1.94 Sc 0.04 Yb 0.02 O 3 The resistivity of the crystal film is 2.32×10 -4 Ω.cm, Hall mobility is 78.33cm 2 / Vs, the carrier concentration is 4.04×10 20 cm -3 .
[0072] Example 5
[0073] Step 1:
[0074] Step A1: ytterbium oxide powder, indium oxide powder and scandium oxide powder are mixed at a molar ratio of indium, scandium and ytterbium of 1.925:0.05:0.025, and then a binder is added, wet-grinded and spray-granulated to obtain a mixed powder;
[0075] Step A2: Pressing the mixed powder into a shape, and then sintering it to obtain a target material of ytterbium oxide doped with indium scandium oxide.
[0076] Step 2:
[0077] Step B1: fixing a target material of ytterbium oxide doped with indium scandium oxide into a target holder of a magnetron sputtering deposition device;
[0078] Step B2: Turn on the RF power supply (sputtering power is 120W) to pre-deposit and clean the target of ytterbium oxide doped indium scandium oxide;
[0079] Step B3: After cleaning, the quartz substrate is fixed on the sample stage, placed in the sputtering chamber and fixed so that the distance between the ytterbium oxide-doped indium scandium oxide target and the quartz substrate is 7 cm;
[0080] The vacuum degree of the growth chamber was evacuated to 3.3×10 -3 Pa, the substrate is heated to 80°C, pure argon gas with a purity of more than 99.99% is introduced, and the pressure is controlled at 0.5Pa;
[0081] Step B4: Turn on the RF power supply again to grow the ytterbium oxide doped indium scandium oxide crystal film on the substrate to a thickness of 100±10nm, and obtain the ytterbium oxide doped indium scandium oxide crystal film. 1.925 Sc 0.05 Yb 0.025 O 3 The resistivity of the crystal film is 3.01×10 -4 Ω.cm, Hall mobility is 75.98cm 2 / Vs, the carrier concentration is 4.06×10 20 cm -3 .
[0082] Example 6
[0083] Step 1:
[0084] Step A1: ytterbium oxide powder, indium oxide powder and scandium oxide powder are mixed at a molar ratio of indium, scandium and ytterbium of 1.91:0.06:0.03, and then a binder is added, and wet grinding and spray granulation are performed to obtain a mixed powder;
[0085] Step A2: Pressing the mixed powder into a shape, and then sintering it to obtain a target material of ytterbium oxide doped with indium scandium oxide.
[0086] Step 2:
[0087] Step B1: fixing a target material of ytterbium oxide doped with indium scandium oxide into a target holder of a magnetron sputtering deposition device;
[0088] Step B2: Turn on the RF power supply (sputtering power is 120W) to pre-deposit and clean the target of ytterbium oxide doped with indium scandium oxide;
[0089] Step B3: After cleaning, the quartz substrate is fixed on the sample stage, placed in the sputtering chamber and fixed so that the distance between the ytterbium oxide-doped indium scandium oxide target and the quartz substrate is 7 cm;
[0090] The vacuum degree of the growth chamber was evacuated to 3.3×10 -3 Pa, the substrate is heated to 80°C, pure argon gas with a purity of more than 99.99% is introduced, and the pressure is controlled at 0.5Pa;
[0091] Step B4: Turn on the RF power supply again to grow the ytterbium oxide doped indium scandium oxide crystal film on the substrate to a thickness of 100±10nm, and obtain the ytterbium oxide doped indium scandium oxide crystal film. 1.91 Sc 0.06 Yb 0.03 O 3 The resistivity of the crystal film is 3.12×10 -4 Ω.cm, Hall mobility is 74.57cm 2 / Vs, the carrier concentration is 4.06×10 20 cm -3 .
[0092] Example 7
[0093] Step 1:
[0094] Step A1: ytterbium oxide powder, indium oxide powder and scandium oxide powder are mixed at a molar ratio of indium, scandium and ytterbium of 1.992:0.004:0.004, and then a binder is added, and wet grinding and spray granulation are performed to obtain a mixed powder;
[0095] Step A2: Pressing the mixed powder into a shape, and then sintering it to obtain a target material of ytterbium oxide doped with indium scandium oxide.
[0096] Step 2:
[0097] Step B1: fixing a target material of ytterbium oxide doped with indium scandium oxide into a target holder of a magnetron sputtering deposition device;
[0098] Step B2: Turn on the RF power supply (sputtering power is 120W) to pre-deposit and clean the target of ytterbium oxide doped with indium scandium oxide;
[0099] Step B3: After cleaning, the quartz substrate is fixed on the sample stage, placed in the sputtering chamber and fixed so that the distance between the ytterbium oxide-doped indium scandium oxide target and the quartz substrate is 6 cm;
[0100] The vacuum degree of the growth chamber was evacuated to 3.3×10-3 Pa, the substrate is heated to 50°C, pure argon gas with a purity of more than 99.99% is introduced, and the pressure is controlled at 0.5Pa;
[0101] Step B4: Turn on the RF power supply again to grow the ytterbium oxide doped indium scandium oxide crystal film on the substrate to a thickness of 100±10nm, and obtain the ytterbium oxide doped indium scandium oxide crystal film. 1.992 Sc 0.004 Yb 0.004 O 3 The resistivity of the crystal film is 3.12×10 -4 Ω.cm, Hall mobility is 81.79cm 2 / Vs, the carrier concentration is 3.28×10 20 cm -3 .
[0102] Example 8
[0103] Step 1:
[0104] Step A1: ytterbium oxide powder, indium oxide powder and scandium oxide powder are mixed at a molar ratio of indium, scandium and ytterbium of 1.992:0.004:0.004, and then a binder is added, and wet grinding and spray granulation are performed to obtain a mixed powder;
[0105] Step A2: Pressing the mixed powder into a shape, and then sintering it to obtain a target material of ytterbium oxide doped with indium scandium oxide.
[0106] Step 2:
[0107] Step B1: fixing a target material of ytterbium oxide doped with indium scandium oxide into a target holder of a magnetron sputtering deposition device;
[0108] Step B2: Turn on the RF power supply (sputtering power is 120W) to pre-deposit and clean the target of ytterbium oxide doped with indium scandium oxide;
[0109] Step B3: After cleaning, the quartz substrate is fixed on the sample stage, placed in the sputtering chamber and fixed so that the distance between the ytterbium oxide-doped indium scandium oxide target and the quartz substrate is 8 cm;
[0110] The vacuum degree of the growth chamber was evacuated to 3.3×10 -3 Pa, the substrate is heated to 100°C, pure argon gas with a purity of more than 99.99% is introduced, and the pressure is controlled at 0.5Pa;
[0111] Step B4: Turn on the RF power supply again to grow the ytterbium oxide doped indium scandium oxide crystal film on the substrate to a thickness of 100±10nm, and obtain the ytterbium oxide doped indium scandium oxide crystal film. 1.992 Sc0.004 Yb 0.004 O 3 The resistivity of the crystal film is 3.14×10 -4 Ω.cm, Hall mobility is 81.91cm 2 / Vs, the carrier concentration is 3.30×10 20 cm -3 .
[0112] Example 9
[0113] Step 1:
[0114] Step A1: ytterbium oxide powder, indium oxide powder and scandium oxide powder are mixed at a molar ratio of indium, scandium and ytterbium of 1.992:0.004:0.004, and then a binder is added, and wet grinding and spray granulation are performed to obtain a mixed powder;
[0115] Step A2: Pressing the mixed powder into a shape, and then sintering it to obtain a target material of ytterbium oxide doped with indium scandium oxide.
[0116] Step 2:
[0117] Step B1: fixing a target material of ytterbium oxide doped with indium scandium oxide into a target holder of a magnetron sputtering deposition device;
[0118] Step B2: Turn on the RF power supply (sputtering power is 120W) to pre-deposit and clean the target of ytterbium oxide doped indium scandium oxide;
[0119] Step B3: After cleaning, the quartz substrate is fixed on the sample stage, placed in the sputtering chamber and fixed so that the distance between the ytterbium oxide-doped indium scandium oxide target and the quartz substrate is 12 cm;
[0120] The vacuum degree of the growth chamber was evacuated to 3.3×10 -3 Pa, the substrate is heated to 70°C, pure argon gas with a purity of more than 99.99% is introduced, and the pressure is controlled at 0.5Pa;
[0121] Step B4: Turn on the RF power supply again to grow the ytterbium oxide doped indium scandium oxide crystal film on the substrate to a thickness of 100±10nm, and obtain the ytterbium oxide doped indium scandium oxide crystal film. 1.992 Sc 0.004 Yb 0.004 O 3 The resistivity of the crystal film is 3.49×10 -4 Ω.cm, Hall mobility is 80.38cm 2 / Vs, the carrier concentration is 3.16×10 20 cm -3 .
[0122] Comparative Example 1
[0123] The same as Example 1, except that titanium oxide is used instead of scandium oxide, and the molar amounts of titanium and scandium are the same, to obtain In 1.992 Ti 0.004 Yb 0.004 O 3 , tested, In 1.992 Ti 0.004 Yb 0.004 O 3 The resistivity of the crystal film is 3.98×10 -4 Ω.cm, Hall mobility is 73.77cm 2 / Vs, the carrier concentration is 3.21×10 20 cm -3 .
[0124] Comparative Example 2
[0125] The same as Example 1, except that terbium oxide is used instead of ytterbium oxide, and the molar amounts of terbium and ytterbium are the same, to obtain In 1.992 Sc 0.004 Tb 0.004 O 3 , tested, In 1.992 Tb 0.004 Yb 0.004 O 3 The resistivity of the crystal film is 4.08×10 -4 Ω.cm, Hall mobility is 73.23cm 2 / Vs, the carrier concentration is 3.17×10 20 cm -3 .
[0126] Comparative Example 3
[0127] The method is basically the same as Example 1, except that the molar ratio of ytterbium oxide powder, indium oxide powder and scandium oxide powder is 1.88:0.08:0.04.
[0128] After testing, 1.88 Sc 0.08 Yb 0.04 O 3 The resistivity of the crystal film is 4.32×10 -4 Ω.cm, Hall mobility is 65.38cm 2 / Vs, the carrier concentration is 4.08×10 20 cm -3 .
[0129] Comparative Example 4
[0130] The method is basically the same as Example 1, except that the molar ratio of ytterbium oxide powder, indium oxide powder and scandium oxide powder is 1.997:0.001:0.0005.
[0131] After testing, 1.9985 Sc 0.001 Yb 0.0005 O 3 The resistivity of the crystal film is 4.07×10 -4 Ω.cm, Hall mobility is 82.78cm 2 / Vs, the carrier concentration is 3.01×10 20 cm -3 .
[0132] Performance Test:
[0133] The conductivity, Hall mobility and carrier concentration of the crystal film were tested by a Hall effect tester. The test results are shown in Table 1:
[0134] Table 1
[0135]
[0136]
[0137] Result analysis:
[0138] 1. It can be seen from Examples 1-6 that when the doping amounts of scandium and ytterbium are gradually increased in Examples 1-6, the carrier concentration of the crystal film shows a trend of gradually increasing, while the Hall mobility shows a trend of gradually decreasing. It can be seen that when ytterbium and scandium elements are doped into indium as the matrix material, the Hall mobility and carrier concentration of the crystal film show a certain inverse relationship;
[0139] At the same time, since both the Hall mobility and the carrier concentration have a crucial influence on the resistivity of the crystal film, the resistivity of Examples 1-6 shows a strong regular change in the carrier concentration and the Hall mobility, while the resistivity does not increase or decrease blindly. It can be seen from Table 1 that when the doping amount of the doping element is less than that of Example 4, the resistivity of Examples 1-3 shows a certain downward trend. When the concentration of the doping element 1 is increased to the concentration of Example 4, the resistivity shows an obvious downward trend. It can be seen that when the doping element reaches the concentration of Example 4 (including Example 4), the influence of the carrier concentration on the resistivity is more significant;
[0140] When the amount of the doping element is greater than that of Example 4, although the carrier concentration of Examples 5-6 is further increased, the resistivity of the crystal film shows a downward trend. It can be seen that when the amount of the doping element is greater than that of Example 4, the influence of the Hall mobility on the resistivity is more significant;
[0141] The effects of the Hall mobility and carrier concentration on the resistivity of Example 4 are just balanced, so that Example 4 achieves a lower resistivity.
[0142] 2. It can be seen from Examples 1 and 7-8 that when the heating temperature of the substrate or the distance between the target and the substrate is changed, when the distance is too small and the heating temperature is too low, on the one hand, the distance is too small, resulting in excessive energy of high-energy particles sputtering onto the target, which is easy to break through the film during the film forming process, thereby reducing the density uniformity and surface roughness of the film, and further reducing the carrier concentration and Hall mobility, resulting in a decrease in the resistivity of Example 7. On the other hand, when the heating temperature is too low, it is more difficult for the unit cells in the crystal film to nucleate, further reducing the density uniformity of the crystal film;
[0143] When the distance is too large, the sputtering energy of high-energy particles decreases. During the film forming process, some particles can be sputtered to the substrate surface, while some cannot, which leads to a decrease in the density uniformity of the film. Higher temperatures cause the unit cells to become too coarse during growth and further reduce the density uniformity of the crystal film, thereby reducing the carrier concentration and Hall mobility.
[0144] Further observation of Example 9 shows that when the distance between the target and the substrate is further increased, it becomes more difficult for the high-energy particles to be completely sputtered to the substrate surface, resulting in a further decrease in the density uniformity of the film;
[0145] 3. It can be seen from Example 1 and Comparative Examples 1-2 that when titanium is used to replace scandium or terbium is used to replace ytterbium, the resistivity of the crystal film will have an upward trend to varying degrees. At the same time, the Hall mobility and carrier concentration of Comparative Examples 1-2 are observed. It can be seen that the Hall mobility and carrier concentration of Comparative Examples 1-2 are reduced to varying degrees relative to Example 1. It can be seen that doping titanium or terbium into an indium-based material cannot effectively increase the carrier concentration as effectively as doping scandium or ytterbium, and will also cause a decrease in Hall mobility;
[0146] 4. It can be seen from Example 1 and Comparative Examples 3-4 that when the doping amount of the doping element is excessively increased or decreased, the resistivity of the crystal film will show a further downward trend.
[0147] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications made without departing from the spirit and principles of the present invention shall be equivalent replacement methods and shall be included in the protection scope of the present invention.
Claims
1. A crystalline thin film of ytterbium oxide doped with indium scandium oxide, characterized in that: The chemical formula of the ytterbium oxide doped indium scandium oxide crystal film is In x Sc y Yb z O3, where 0.002≤y≤0.06, 0.001≤z≤0.03, and x+y+z=2.
2. The ytterbium oxide doped indium scandium oxide crystal thin film according to claim 1, characterized in that: The chemical formula of the ytterbium oxide doped indium scandium oxide crystal film is In x Sc y Yb z O3, wherein 0.01≤y≤0.05, 0.01≤z≤0.025, and x+y+z=2.
3. The ytterbium oxide doped indium scandium oxide crystal thin film according to claim 1, characterized in that: The chemical formula of the ytterbium oxide doped indium scandium oxide crystal film is In x Sc y Yb z O3, where y=0.04, z=0.02, and x+y+z=2.
4. A method for preparing a crystalline thin film of ytterbium oxide doped with indium scandium oxide as claimed in any one of claims 1 to 3, characterized in that: The following steps are involved: Step 1: Mixing, pressing and sintering ytterbium oxide powder, indium oxide powder and scandium oxide powder to obtain a target material of ytterbium oxide doped with indium oxide and scandium oxide; Step 2: Deposit the ytterbium oxide doped indium scandium oxide target material obtained in step 1 onto an external substrate to obtain a crystalline film of ytterbium oxide doped indium scandium oxide.
5. The method for preparing a crystalline thin film of ytterbium oxide doped with indium scandium oxide according to claim 4, characterized in that: The step 1 comprises the following sub-steps: Step A1: mixing ytterbium oxide powder, indium oxide powder and scandium oxide powder, then adding a binder, wet grinding and spray granulation to obtain a mixed powder; Step A2: Pressing the mixed powder into a shape, and then sintering it to obtain a target material of ytterbium oxide doped with indium scandium oxide.
6. The method for preparing a crystalline thin film of ytterbium oxide doped with indium scandium oxide according to claim 4, characterized in that: In the step 2, the deposition method of depositing the target material of ytterbium oxide doped with indium scandium oxide onto the substrate of the external device is magnetron sputtering.
7. The method for preparing a crystalline thin film of ytterbium oxide doped with indium scandium oxide according to claim 6, characterized in that: The step 2 includes the following sub-steps: Step B1: fixing a target material of ytterbium oxide doped with indium scandium oxide into a target holder of a magnetron sputtering deposition device; Step B2: Turn on the radio frequency power supply to pre-deposit and clean the target material of ytterbium oxide doped indium scandium oxide; Step B3: Then, the substrate is fixed on the sample stage, placed in the sputtering chamber, and the substrate is heated to 50-100° C. in a vacuum environment; Step B4: Turn on the radio frequency power supply again to grow the crystalline film of ytterbium oxide doped with indium scandium oxide on the substrate to a thickness of 100±10 nm, thereby obtaining the crystalline film of ytterbium oxide doped with indium scandium oxide.
8. The method for preparing a crystalline thin film of ytterbium oxide doped with indium scandium oxide according to claim 7, characterized in that: In the step B3, the distance between the target material of ytterbium oxide doped with indium scandium oxide and the substrate is 6 to 8 cm.
Citation Information
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