A method for defect configuration of c-axis preferentially oriented AlN thin film for high temperature temperature measurement

Abstract

The present application belongs to the technical field of temperature measurement, especially high-temperature temperature measurement, and specifically provides a defect construction method of C-axis preferred orientation AlN film for high-temperature temperature measurement, to improve temperature interpretation accuracy. The present application uses a medium-frequency reactive magnetron sputtering method to realize the preparation of C-axis preferred orientation AlN film, and in the sputtering process, uniform and controllable lattice defects are constructed in the C-axis preferred orientation AlN film through the method of active gas doping. The lattice defect construction method provided by the present application is simple in process, good in stability and repeatability, does not need neutron irradiation, and is low in cost. The C-axis preferred orientation AlN film with uniform and controllable lattice defects as a temperature sensitive material can realize high-temperature temperature measurement and improve temperature interpretation accuracy.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of temperature measurement, especially high-temperature temperature measurement, and particularly provides a defect construction method of a C-axis preferred orientation AlN film for high-temperature temperature measurement. BACKGROUND

[0002] The surface temperature, strain and other state parameter distribution of the hot end components of an aero-engine, a rocket engine, a ship and an industrial gas turbine have an important influence on the performance and service life of the components. Meanwhile, in order to evaluate the effectiveness of thermal-mechanical modeling and simulation and verify the effectiveness of the film cooling technology and the thermal barrier coating technology, it is very important to accurately measure the temperature and other parameter distribution of the components under the working condition.

[0003] At present, as the working temperature of the hot end components is higher and higher, higher requirements are put forward for the surface temperature test of the components, and distributed accurate test is required. The neutron irradiation crystal temperature measurement has the advantages of no need of lead, high temperature measurement accuracy, many points of distribution, wide temperature measurement range and the like, and is an advanced technology for measuring the surface temperature field of the hot end components. The temperature measurement principle of the neutron irradiation crystal temperature measurement method is that the single crystal material (such as SiC, AlN, diamond and the like) causes internal displacement defects after receiving high-dose neutron irradiation. The defects will occur a certain degree of recovery after annealing at a specific temperature, and the recovery degree is approximately linearly related to the high-temperature temperature history. Moreover, the defect recovery degree does not change with the decrease of the temperature, that is, the defect recovery degree has a memory effect on the highest temperature experienced by the crystal. The recovery degree of the defects can be accurately tested by measuring the crystal lattice parameters. Based on this, by using the temperature memory effect, a calibration curve of the crystal lattice parameters and the highest annealing temperature is established through a temperature calibration experiment, and then the crystal lattice parameters of the material after service are measured to inversely deduce the highest temperature in the service process, so as to accurately test the surface temperature of the hot end components. However, the single crystal material needs to be neutron irradiated in advance, the neutron irradiation cost is high, the irradiation period is long, and the construction process is complex when used, such as hole opening and embedding on the surface of the blade. In addition, in the Chinese invention patent with the patent number ZL201810366196.4, a temperature measurement method using a C-axis oriented AlN film as a sensor, the residual defect concentration of the AlN film is represented by the half-peak width or the peak position of the XRD diffraction peak, and the evolution rule of the intrinsic defects in the AlN film with temperature is used as the basis for temperature measurement, so as to realize the temperature interpretation. However, the concentration of the repairable intrinsic defects in the directly deposited C-axis preferred orientation AlN film is not high, which leads to low accuracy of the temperature interpretation result. Therefore, in order to improve the temperature interpretation accuracy, how to construct the impurity defects repairable with temperature in the AlN film becomes the research focus of the application. SUMMARY

[0004] The application aims to provide a C-axis preferred orientation AlN film defect construction method for high-temperature temperature measurement, so as to improve temperature judgment accuracy.

[0005] To achieve the above object, the technical scheme adopted by the application is:

[0006] A C-axis preferred orientation AlN film defect construction method for high-temperature temperature measurement, characterized in that it comprises the following steps:

[0007] An Al target with a purity greater than 99.99wt% is used as a sputtering target material, and a mixture of nitrogen and active gas is used as a reaction gas, wherein the volume fraction of the active gas is 1% to 4%;

[0008] The parameters are set as follows: a back background vacuum degree of 5 to 8*10 -4 Pa, a sputtering power of 1000 to 3000W, a sputtering gas pressure of 0.4 to 2.0Pa, and a deposition temperature of normal temperature to 300℃;

[0009] A C-axis preferred orientation AlN film is deposited and grown on a substrate by a medium-frequency reaction magnetron sputtering method, and the C-axis preferred orientation AlN film grown has crystal defects.

[0010] Further, the active gas is hydrogen or methane.

[0011] Further, the thickness of the C-axis preferred orientation AlN film is 100nm to 5μm.

[0012] Further, the crystal defects of the C-axis preferred orientation AlN film include point defects, line defects, surface defects and bulk defects.

[0013] Further, the substrate is an alumina ceramic sheet, a quartz sheet, a sapphire or an alloy sheet, and the substrate thickness is 50μm to 1mm.

[0014] A temperature sensitive material for high-temperature temperature measurement, characterized in that the temperature sensitive material is a C-axis preferred orientation AlN film with crystal defects prepared by the above C-axis preferred orientation AlN film defect construction method for high-temperature temperature measurement, and the temperature measurement range is 400 to 1400℃.

[0015] The application provides a C-axis preferred orientation AlN film defect construction method for high-temperature temperature measurement. Figure 1 As shown in the figure, the temperature reading accuracy is improved, and the cost of the crystal temperature measurement technology is reduced and the temperature measurement process is simplified.

[0016] Based on the above technical solutions and working principles, the application has the following advantages:

[0017] 1) The application provides a C-axis preferred orientation AlN film defect construction method for high-temperature temperature measurement, which improves the defect concentration of the C-axis preferred orientation AlN film by active gas doping, effectively improves the resolution, temperature measurement accuracy and temperature measurement range of the temperature measurement data.

[0018] 2) The C-axis preferred orientation AlN film containing a large number of defects in the application can be used as a sensitive material for temperature testing. The lattice defect construction method provided by the application is simple in process, good in stability and repeatability, does not need neutron irradiation, and is low in cost. The lattice defects constructed in the C-axis preferred orientation AlN film are uniform and controllable. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 The application provides a principle diagram for lattice defect construction and repair in the C-axis preferred orientation AlN film. DETAILED DESCRIPTION

[0020] In order to make the purpose, technical scheme and advantages of the application clearer, the application is further described in detail below with reference to the drawings and examples.

[0021] Example 1

[0022] The application provides a C-axis preferred orientation AlN film defect construction method, and the C-axis preferred orientation AlN film with uniform and controllable lattice defects prepared by the method can be used as a temperature measurement sensitive material, realizes high-temperature temperature measurement, and effectively improves the temperature reading accuracy. The C-axis preferred orientation AlN film defect construction method specifically includes the following steps:

[0023] Quartz wafers are used as substrates, and the substrates are sequentially cleaned with acetone, anhydrous ethanol and deionized water for 15 minutes, and then dried for use;

[0024] The Al target with purity greater than 99.99wt% is used as a sputtering target, and the mixed gas of nitrogen and hydrogen is used as a reaction gas, wherein the volume fraction of hydrogen is 4%;

[0025] The setting parameters are as follows: the background vacuum degree is 5*10 -4 Pa, the sputtering power is 2000W, the sputtering pressure is 0.8Pa, and the deposition temperature is 300℃.

[0026] The C-axis preferred orientation AlN film with a thickness of 2.7μm is deposited and grown on a substrate by a medium-frequency reactive magnetron sputtering method, and the C-axis preferred orientation AlN film has crystal defects.

[0027] Further, the H-ion doped C-axis preferred orientation AlN film prepared above is subjected to isochronal annealing treatment at temperatures of 400℃, 500℃, 600℃, 700℃, 800℃ and 900℃, and the annealing time is 5min, 10min and 15min; then the diffraction angle 2θ of the (002) crystal plane of the AlN film after the annealing treatment is tested by X-ray diffraction technology, the high-temperature annealing makes the H-ion leave the aluminum nitride film, and part of the defects is repaired, so that the crystal lattice of the AlN film shrinks, the XRD diffraction angle increases, and the diffraction angle increases approximately linearly with the increase of temperature and time, thereby establishing the relationship between the diffraction angle 2θ and the annealing temperature and time as the basis for temperature interpretation, and realizing high-temperature temperature measurement.

[0028] In the process of sputtering the AlN film, the H2 is added to construct a uniform and controllable crystal lattice defect, the H-ion doping causes a large number of crystal lattice defects in the AlN film, the defects cause the crystal lattice to stretch, so that the (002) crystal plane diffraction angle of the AlN film becomes smaller, and the higher the volume fraction of the H2 introduced, the higher the degree of lattice distortion of the AlN film, and the smaller the (002) crystal plane diffraction angle. Compared with the problems of being indispensable in the neutron irradiation process in the SiC crystal temperature measurement technology, high processing difficulty and high cost, the defect construction process of the present application is simple and low in cost, the H-ion doped C-axis preferred orientation AlN film prepared has a temperature memory effect, and the highest temperature experienced by the film can be inferred by using the linear change relationship between the crystal structure parameter 2θ of the AlN film and the annealing temperature and time.

[0029] Example 2

[0030] The present embodiment provides a C-axis preferred orientation AlN film defect construction method, comprising the following steps:

[0031] A quartz piece is used as a substrate, and the substrate is sequentially ultrasonically cleaned with acetone, anhydrous ethanol and deionized water for 15min, and then dried for use;

[0032] The Al target with a purity of greater than 99.99wt% is used as a sputtering target, and the mixed gas of nitrogen and methane is used as a reaction gas, wherein the volume fraction of methane is 1%.

[0033] The setting parameters are as follows: the background vacuum degree is 5*10 -4 Pa, the sputtering power is 2000W, the sputtering pressure is 0.8Pa, and the deposition temperature is 300℃.

[0034] The C-axis preferred orientation AlN film with a thickness of 2.7μm is deposited and grown on a substrate by a medium-frequency reaction magnetron sputtering method, and the C-axis preferred orientation AlN film has crystal defects.

[0035] Further, the H-ion doped C-axis preferred orientation AlN film prepared above is subjected to isochronal annealing treatment at temperatures of 700℃, 800℃, 900℃, 1000℃ and 1100℃, and the annealing time is 5min and 10min; then the diffraction angle 2θ of the (002) crystal plane of the AlN film after annealing treatment is tested by X-ray diffraction technology, the high-temperature annealing also repairs part of the defects of the AlN film, so that the crystal lattice of the AlN film shrinks, the XRD diffraction angle increases, and the diffraction angle increases approximately linearly with the increase of temperature and also increases approximately linearly with the increase of time, thereby establishing the relationship between the diffraction angle 2θ and the annealing temperature and the annealing time as the basis for temperature interpretation, and realizing high-temperature temperature measurement.

[0036] The CH4 doped C-axis preferred orientation AlN film prepared in the embodiment also has a temperature memory effect, and the linear change relationship between the crystal structure parameter 2θ of the AlN film and the annealing temperature and the annealing time can be used to infer the highest temperature experienced by the film.

[0037] The above is only a specific embodiment of the present application, any feature disclosed in the specification can be replaced by other equivalent or similar purpose alternative features unless specifically described, and all features disclosed or all steps in the method or process can be combined in any way except for mutually exclusive features and / or steps.

Claims

1. A method for defect formation of C-axis preferentially oriented AlN thin film for high temperature temperature measurement, characterized by, The method comprises the following steps: The Al target with a purity of more than 99.99wt% is used as a sputtering target material, and the mixed gas of nitrogen and active gas is used as a reaction gas, wherein the volume fraction of the active gas is 1% to 4%, and the active gas is hydrogen or methane; Setting parameters: background vacuum degree is 5~8×10 -4 Pa, sputtering power is 1000~3000W, sputtering pressure is 0.4~2.0Pa, and deposition temperature is normal temperature~300℃; The C-axis preferred orientation AlN film is deposited on the substrate by a medium-frequency reactive magnetron sputtering method, and the C-axis preferred orientation AlN film has crystal defects after growth, the crystal defects are uniform and controllable and can be repaired with temperature, and the crystal defects of the C-axis preferred orientation AlN film include point defects, line defects, surface defects and bulk defects.

2. The method for defect formation of C-axis preferentially oriented AlN thin film for high temperature temperature measurement according to claim 1, wherein The thickness of the C-axis preferred orientation AlN film is 100nm to 5μm.

3. The method for defect formation of C-axis preferentially oriented AlN thin film for high temperature temperature measurement according to claim 1, wherein The substrate is an alumina ceramic sheet, a quartz sheet, sapphire, a mica sheet or an alloy sheet, and the thickness of the substrate is 50μm to 1mm.

4. A temperature sensitive material for high temperature temperature measurement, characterized in that, The temperature sensitive material is the C-axis preferred orientation AlN film with crystal defects prepared by the method for preparing a C-axis preferred orientation AlN film defect structure for high-temperature temperature measurement, and the temperature measurement range of the temperature sensitive material is 400 to 1400℃.

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