Thin film type integrated temperature control chip material and preparation method thereof

Abstract

The invention provides a film type integrated temperature control chip material and a preparation method thereof, the film type integrated temperature control chip material is composed of a substrate, an insulating buffer layer, a heating film, a thermosensitive film, an interdigital electrode, a terminal electrode and an insulating layer, and the insulating buffer layer, the heating film, the thermosensitive film, the electrode and the insulating layer are grown on the substrate. Different functional films grow in a composite mode to form the integrated temperature control chip. And the heating performance and the temperature measurement sensitivity are regulated and controlled by adjusting the types and growth preparation conditions of the films. The film type integrated temperature control chip material is simple in structure, light and thin in mass, good in film crystallinity, small in roughness and high in temperature sensitivity. Through compatibility of a coating process and a semiconductor process, the process of converting the film from basic research to practical research is realized. The problem that a heater and a thermistor are separated in the prior art is solved, and a heating film and a negative temperature coefficient temperature measurement film are organically integrated together, so that the temperature measurement precision is effectively improved. And meanwhile, the application channel of the device is widened due to the small size.

Description

Technical Field

[0001] The present invention relates to the field of preparation of two-dimensional materials and temperature sensor integration, and in particular to a thin-film integrated temperature control chip material and a preparation method thereof. Background Art

[0002] As a real-time temperature measurement device, temperature sensor is the main way and means to obtain information in the modern information society, and plays an indispensable role in people's production and life. As my country turns to the direction of the Internet of Things and digitalization, the research on integrated intelligent temperature sensors with thermosensitive film as the core has gradually become a hot topic. Temperature sensors are divided into active and passive sensors. Active sensors can send certain detection signals to the object being measured, detect the changes caused by the detection signal in the object being measured, or form signals by the detection signal producing a certain effect in the object being measured. Radar and radio frequency range detectors are action-type examples, while photoacoustic effect analysis devices and laser analyzers are reaction-type examples. Passive sensors only receive signals generated by the object being measured, such as infrared radiation thermometers, infrared cameras, etc. In the face of increasingly complex environmental interference, passive temperature sensors have more limitations, while active temperature sensors have better flexibility. However, most of the existing active temperature sensors are combined by bonding micro heaters and thermistors. In actual use, they have complex preparation, high cost, and difficulty in measuring temperature in a small space.

[0003] In order to solve the above problems, the present invention proposes a method for preparing a thin film integrated temperature control chip based on the original heating film. The method uses the integrated growth method of two-dimensional NTC thermistor film and two-dimensional heating material to grow multiple functional materials on the substrate surface and integrate them by bonding, which not only avoids the problem of large volume and high cost, but also improves the sensitivity and reliability of temperature measurement. Summary of the invention

[0004] The object of the present invention is to provide a thin film type integrated temperature control chip material and preparation method, the method is composed of a substrate, an insulating buffer layer, a heating film, a thermosensitive film, a forked electrode, an end electrode and an insulating layer, an insulating buffer layer, a heating film, an NTC thermosensitive film, an electrode and an insulating layer are grown on the substrate, and different functional films are grown in a composite manner to form an integrated temperature control chip. By adjusting the type of film and the growth preparation conditions, the heating performance and temperature measurement sensitivity can be regulated. The thin film type integrated temperature control chip has a simple structure, a light weight, and a good crystallinity of the film, a small roughness, and a high sensitivity to temperature. Through the compatibility of the coating process and the semiconductor process, the process of transforming the film from basic research to practical research is realized. The present invention solves the problem of separation between the heater and the thermistor in the prior art, and organically integrates the heating film and the NTC temperature measurement film, so that the temperature measurement accuracy is effectively improved. At the same time, the smaller volume also broadens its application channels. Through structural design and material selection, the present invention adopts NTC-based thermosensitive film to effectively improve the temperature control accuracy on the one hand; on the other hand, adopts a new structural design to reduce the cost and size of the temperature control chip, which is convenient for flexible application in multiple fields.

[0005] The present invention discloses a thin-film integrated temperature control chip material, which comprises a substrate (1), an insulating buffer layer (2), a heating film (3), a thermosensitive film (4), interdigital electrodes (5), terminal electrodes (6) and an insulating layer (7). An insulating buffer layer (2), a heating film (3), a thermosensitive film (4), interdigital electrodes (5) and terminal electrodes (6) are respectively arranged between the substrate (1) and the insulating layer (7). A thermosensitive film (4) is arranged on one side of the surface of the insulating buffer layer (2), and a heating film (3) is arranged on the other side. Terminal electrodes (6) are respectively arranged at both ends of the surface of the heating film (3), and an interdigital electrode (5) is arranged on the surface of the thermosensitive film (4). The specific operation is performed according to the following steps:

[0006] a. Substrate cleaning: ultrasonically cleaning the substrate (1) with acetone, anhydrous ethanol, deionized water and anhydrous ethanol respectively, with the cleaning time being 10-30 minutes respectively, and blowing the surface of the substrate (1) dry with high-purity dry nitrogen after cleaning, wherein the substrate (1) is silicon oxide, silicon nitride, aluminum oxide, aluminum nitride, alloy material or fluorphlogopite, and the substrate size is 0.1-6 inches;

[0007] b. Preparation of buffer layer: SrTiO3, BaTiO3, SrZrO3, BaZrO3, Al2O3, AlN, SiO2 or Si3N4 are selected as the insulating buffer layer (2) material, and the substrate (1) obtained in step a is subjected to DC magnetron sputtering to grow the insulating buffer layer (2). The RF sputtering conditions are: the growth pressure is 10 -1-10Pa, oxygen and argon contents are 0%-100% respectively, growth power is 10-80W, growth temperature is 50-500°C, growth time is 60-600min, annealing treatment is carried out in a tube furnace, annealing temperature is 300-600°C, heating time is 1-10°C / min, holding time is 10-60min, cooling time is 1-10°C / min, annealing atmosphere is air, oxygen, nitrogen, argon or hydrogen, and insulating buffer layer (2) is obtained;

[0008] c. Preparation of the heating layer: Tantalum nitride, copper-nickel alloy, nickel-chromium alloy, iron-chromium-aluminum alloy, and platinum materials are selected as the heating film (3) material. The substrate (1) with the insulating buffer layer (2) obtained in step b is used for growing the heating film (3) by DC magnetron sputtering. A mask is used to cover 1 / 3 of the surface of the insulating buffer layer (2), and sputtering is carried out on the remaining 2 / 3. The sputtering conditions are: the growth pressure is 10 -1 -10Pa, oxygen and argon contents are 0%-100% respectively, growth power is 10-80W, growth temperature is 50-500°C, growth time is 20-120min, annealing treatment is carried out in a tube furnace, annealing temperature is 300-600°C, heating time is 1-10°C / min, holding time is 10-60min, cooling time is 1-10°C / min, annealing atmosphere is air, oxygen, nitrogen, argon or hydrogen, and a heated film (3) material is obtained;

[0009] d. Preparation of negative temperature coefficient thermistor film: MnCoNiO or LaMnO materials are selected as the thermosensitive film (4) material, the heating film (3) material prepared in step c is placed in a magnetron sputtering device to grow a negative temperature coefficient thermistor film, 2 / 3 of the prepared heating film (3) is covered with a mask, and the remaining 1 / 3 is sputtered. The sputtering conditions are: the growth pressure is 10 -1 -10Pa, oxygen and argon contents are 0%-100% respectively, growth power is 10-80W, growth temperature is 50-500°C, growth time is 20-120min, annealing treatment is carried out in a tube furnace, annealing temperature is 300-1000°C, heating time is 1-10°C / min, holding time is 10-60min, cooling time is 1-10°C / min, annealing atmosphere is air, oxygen, nitrogen, argon or hydrogen, and negative temperature coefficient thermistor film (4) material is obtained;

[0010] e. Electrode preparation: The heating film (3) material obtained in step c and the negative temperature coefficient thermistor (4) layer obtained in step d are covered with electrode masks respectively, and are placed in the tray of the DC sputtering device again to prepare Cr / Au or Ni / Au electrodes according to the conventional method. In this process, the heating film (3) material and the negative temperature coefficient thermistor (4) material are covered with electrode masks respectively, and the growth power is 10-50W and the growth pressure is 10 -1 -10Pa, the growth time of the two materials is 3-15min respectively. After the growth is completed, they are placed in an oven for annealing at a temperature of 125-250°C for 1-4h. After the annealing is completed, an integrated heating and temperature measurement composite film is obtained;

[0011] f. Preparation of insulating protective layer: Bonding and leading out leads on the surface of the integrated heating and temperature measuring composite film obtained in step e, and coating the surface with an insulating layer (7) as a packaging and protective layer, Al2O3, AlN, SiO2 or Si3N4 are selected as the insulating layer (7) material, and the RF sputtering vacuum degree is 2×10 -3 -2×10 -5 Pa, the growth pressure is 10 -1 -10Pa, oxygen and argon content are 0%-100% respectively, growth power is 10-80W, growth temperature is 50-500℃, growth time is 60-600min, annealing treatment is carried out in a tubular furnace, annealing temperature is 300-600℃, heating time is 1-10℃ / min, holding time is 10-60min, cooling time is 1-10℃ / min, annealing atmosphere is air, oxygen, nitrogen, argon or hydrogen, and a thin film integrated temperature control chip is obtained.

[0012] The thin-film integrated temperature control chip material and preparation method described in the present invention are characterized by:

[0013] The present invention prepares and applies both the heating module and the temperature measuring module in the form of thin films, thereby avoiding the problems of poor bonding between the two, large volume and high cost.

[0014] The present invention adopts a magnetron sputtering method to prepare the functional layer material, and can achieve performance optimization according to a simple change in process parameters, with better film uniformity and higher temperature measurement accuracy. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 This is a schematic diagram of the internal structure of the integrated temperature control chip of the present invention;

[0016] Figure 2 This is a schematic diagram of the integrated temperature control chip of the present invention;

[0017] Figure 3 This is a graph showing how the resistance of the integrated temperature control chip of the present invention changes with temperature. DETAILED DESCRIPTION

[0018] The present invention and its effective technical effects are further described in detail below in conjunction with examples and drawings, but the embodiments of the invention are not limited thereto. Any modification or equivalent substitution of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention should be included in the protection scope of the present invention.

[0019] Example 1

[0020] The present invention discloses a thin film integrated temperature control chip material, which is composed of a substrate 1, an insulating buffer layer 2, a heating film 3, a thermosensitive film 4, an interdigital electrode 5, an end electrode 6 and an insulating layer 7. The insulating buffer layer 2, the heating film 3, the thermosensitive film 4, the interdigital electrode 5 and the end electrode 6 are respectively arranged between the substrate 1 and the insulating layer 7. The thermosensitive film 4 is arranged on one side of the surface of the insulating buffer layer 2, and the heating film 3 is arranged on the other side. The end electrodes 6 are respectively arranged at both ends of the surface of the heating film 3, and the interdigital electrode 5 is arranged on the surface of the thermosensitive film 4. The specific operation is performed according to the following steps:

[0021] a. Substrate cleaning: A 2-inch silicon oxide substrate 1 was ultrasonically cleaned with acetone, anhydrous ethanol, deionized water and anhydrous ethanol respectively, with each cleaning time being 10 minutes. After cleaning, the surface of the substrate 1 was blown dry with high-purity dry nitrogen;

[0022] b. Preparation of buffer layer: SrTiO3 is selected as the material of the insulating buffer layer 2, and the silicon oxide substrate 1 obtained in step a is grown by DC magnetron sputtering. The RF sputtering conditions are: the growth pressure is 10 -1 Pa, oxygen content of 50%, argon content of 100%, growth power of 40W, growth temperature of 150°C, growth time of 360min, annealing treatment in a tube furnace, annealing temperature of 400°C, heating time of 5°C / min, holding time of 60min, cooling time of 5°C / min, annealing atmosphere of air, to obtain an insulating buffer layer 2;

[0023] c. Preparation of heating layer: Tantalum nitride is selected as the material of heating film 3, and the silicon oxide substrate 1 with insulating buffer layer 2 obtained in step b is used for growing heating film 3 by DC magnetron sputtering, and a mask is used to cover 1 / 3 of the surface of insulating buffer layer 2, and sputtering is carried out on the remaining 2 / 3. The sputtering conditions are: growth pressure of 1Pa, oxygen content of 0%, argon content of 100%, growth power of 50W, growth temperature of 200°C, growth time of 120min, and annealing treatment is carried out in a tube furnace, the annealing temperature is 400°C, the heating time is 5°C / min, the holding time is 30min, the cooling time is 1°C / min, and the annealing atmosphere is nitrogen, so as to obtain heating film 3 material;

[0024] d. Preparation of negative temperature coefficient thermistor film: MnCoNiO material is selected as the material of the thermosensitive film 4, and the heating film 3 material prepared in step c is placed in a magnetron sputtering device for negative temperature coefficient thermistor film growth, and the prepared 2 / 3 part of the heating film 3 is covered with a mask, and then the remaining 1 / 3 part is sputtered, and the sputtering conditions are: growth pressure is 1Pa, oxygen content is 0%, argon content is 100%, growth power is 50W, growth temperature is 200℃, growth time is 20min, annealing treatment is carried out in a tube furnace, annealing temperature is 800℃, heating time is 10℃ / min, holding time is 30min, cooling time is 10℃ / min, annealing atmosphere is air, and negative temperature coefficient thermistor film 4 material is obtained;

[0025] e. Electrode preparation: The surfaces of the heating film 3 material obtained in step c and the negative temperature coefficient thermistor film 4 obtained in step c are covered with electrode masks respectively, and are placed in the tray of the DC sputtering equipment again to prepare Cr / Au electrodes according to the conventional method. In this process, the heating film 3 material and the negative temperature coefficient thermistor film 4 material are partially covered with electrode masks respectively. The growth power is 40W, the growth pressure is 1Pa, and the growth time of the two materials is 3min and 15min respectively. After the growth is completed, they are placed in an oven for annealing at a temperature of 125°C for 4h. After the annealing is completed, an integrated heating and temperature measurement composite film is obtained;

[0026] f. Preparation of insulating protective layer: Bond the surface of the integrated heating and temperature measuring composite film obtained in step e and lead out the leads, and coat the surface with Al2O3 as an insulating layer 7 as a packaging and protective layer. The RF sputtering vacuum degree is 2×10 -5Pa, the growth gas pressure is 1Pa, the oxygen content is 0%, the argon content is 100%, the growth power is 40W, the growth temperature is 150℃, the growth time is 300min, and annealing treatment is carried out in a tubular furnace, the annealing temperature is 450℃, the heating time is 10℃ / min, the holding time is 45min, the cooling time is 5℃ / min, and the annealing atmosphere is oxygen, so as to obtain a thin film integrated temperature control chip material.

[0027] Example 2

[0028] The material composition of the thin film integrated temperature control chip is based on Example 1, and the specific operation is carried out according to the following steps:

[0029] a. Substrate cleaning: A 0.1-inch silicon nitride substrate 1 is ultrasonically cleaned with acetone, anhydrous ethanol, deionized water and anhydrous ethanol respectively, with the cleaning time being 15 minutes each. After cleaning, the surface of the silicon nitride substrate 1 is blown dry with high-purity dry nitrogen;

[0030] b. Preparation of buffer layer: BaTiO3 is selected as the insulating buffer layer 2 material, and the silicon nitride substrate 1 obtained in step a is subjected to DC magnetron sputtering to grow the insulating buffer layer 2. The RF sputtering conditions are: the growth pressure is 10 -1 Pa, oxygen content 0%, argon content 10%, growth power 10W, growth temperature 50°C, growth time 60min, annealing treatment in a tube furnace, annealing temperature 300°C, heating time 1°C / min, holding time 10min, cooling time 1°C / min, annealing atmosphere is air, and insulating buffer layer 2 is obtained;

[0031] c. Preparation of heating layer: copper-nickel alloy is selected as the material of heating film 3, and the silicon oxide substrate 1 with insulating buffer layer 2 obtained in step b is used for growing heating film 3 by DC magnetron sputtering. A mask is used to cover 1 / 3 of the surface of insulating buffer layer 2, and sputtering is carried out on the remaining 2 / 3. The sputtering conditions are: the growth pressure is 10 -1 Pa, oxygen content and argon content are 0% respectively, growth power is 10W, growth temperature is 50°C, growth time is 20min, annealing treatment is carried out in a tube furnace, annealing temperature is 300°C, heating time is 1°C / min, holding time is 10min, cooling time is 1°C / min, annealing atmosphere is air, and heating film 3 material is obtained;

[0032] d. Preparation of negative temperature coefficient thermistor film: LaMnO series material is selected as the material of the thermosensitive film 4, and the heating film 3 material prepared in step c is placed in a magnetron sputtering device for negative temperature coefficient thermistor film growth, and the prepared 2 / 3 part of the heating film 3 is covered with a mask, and then the remaining 1 / 3 part is sputtered. The sputtering conditions are: the growth pressure is 10 -1 Pa, oxygen and argon content are 0%, growth power is 10W, growth temperature is 50℃, growth time is 20min, annealing treatment is carried out in a tube furnace, annealing temperature is 300℃, heating time is 1℃ / min, holding time is 10min, cooling time is 1℃ / min, annealing atmosphere is air, and negative temperature coefficient thermistor film 4 material is obtained;

[0033] e. Electrode preparation: The heating film 3 material obtained in step c and the negative temperature coefficient thermistor film 4 obtained in step d are covered with electrode masks respectively, and are placed in the tray of the DC sputtering equipment again to prepare Ni / Au electrodes according to the conventional method. In this process, the heating film 3 material and the negative temperature coefficient thermistor film 4 material are partially covered with electrode masks respectively, and the growth power is 10W and the growth pressure is 10 -1 Pa, the growth time of the two materials is 3min respectively. After the growth is completed, they are placed in an oven for annealing at a temperature of 125℃ for 1h. After the annealing is completed, an integrated heating and temperature measurement composite film is obtained;

[0034] f. Preparation of insulating protective layer: Bond the surface of the integrated heating and temperature measuring composite film obtained in step e and lead out the leads, and coat the surface with AlN as an insulating layer 7 as a packaging and protective layer. The RF sputtering vacuum degree is 2×10 -3 Pa, the growth pressure is 10 -1 Pa, oxygen and argon content are 0% respectively, the growth power is 10W, the growth temperature is 50℃, the growth time is 60min, and annealing treatment is carried out in a tubular furnace. The annealing temperature is 300℃, the heating time is 1℃ / min, the insulation time is 10min, the cooling time is 1℃ / min, and the annealing atmosphere is nitrogen, so as to obtain a thin film integrated temperature control chip material.

[0035] Example 3

[0036] The material composition of the thin film integrated temperature control chip is based on Example 1, and the specific operation is carried out according to the following steps:

[0037] a. Substrate cleaning: ultrasonically clean the 6-inch alloy substrate 1 with acetone, anhydrous ethanol, deionized water and anhydrous ethanol respectively, with each cleaning time being 20 minutes. After cleaning, the surface of the alloy substrate 1 is blown dry with high-purity dry nitrogen;

[0038] b. Preparation of buffer layer: SrZrO3 is selected as the material of the insulating buffer layer 2, and the alloy material substrate 1 obtained in step a is subjected to DC magnetron sputtering to grow the insulating buffer layer 2, and the RF sputtering conditions are: growth pressure is 10Pa, oxygen and argon content are 100% respectively, growth power is 80W, growth temperature is 500°C, growth time is 600min, annealing treatment is carried out in a tubular furnace, annealing temperature is 600°C, heating time is 10°C / min, holding time is 60min, cooling time is 10°C / min, annealing atmosphere is nitrogen, and the insulating buffer layer 2 is obtained;

[0039] c. Preparation of heating layer: nickel-chromium alloy is selected as the material of heating film 3, and the substrate 1 with insulating buffer layer 2 obtained in step b is used for growing heating film 3 by DC magnetron sputtering, and a mask is used to cover 1 / 3 of the surface of insulating buffer layer 2, and sputtering is carried out on the remaining 2 / 3. The sputtering conditions are: growth pressure is 10Pa, oxygen and argon content are 100% respectively, growth power is 80W, growth temperature is 500℃, growth time is 120min, annealing treatment is carried out in a tube furnace, annealing temperature is 600℃, heating time is 10℃ / min, holding time is 60min, cooling time is 10℃ / min, annealing atmosphere is air, and heating film 3 material is obtained;

[0040] d. Preparation of negative temperature coefficient thermistor film: MnCoNiO-based material is selected as the material of the thermosensitive film 4, and the heating film 3 material prepared in step c is placed in a magnetron sputtering device for negative temperature coefficient thermistor film growth, and the prepared 2 / 3 part of the heating film 3 is covered with a mask, and then the remaining 1 / 3 part is sputtered, and the sputtering conditions are: growth pressure is 10Pa, oxygen and argon content are 100% respectively, growth power is 80W, growth temperature is 500℃, growth time is 120min, annealing treatment is carried out in a tube furnace, annealing temperature is 1000℃, heating time is 10℃ / min, insulation time is 60min, cooling time is 10℃ / min, annealing atmosphere is air, and negative temperature coefficient thermistor film 4 material is obtained;

[0041] e. Electrode preparation: The surfaces of the heating film 3 material obtained in step c and the negative temperature coefficient thermistor film 4 obtained in step d are respectively covered with electrode masks, and are placed in a tray of a DC sputtering device again to prepare a Cr / Au electrode in a conventional manner. In this process, the heating film (3) material and the negative temperature coefficient thermistor film (4) material are respectively covered with electrode masks. The growth power is 50 W, the growth pressure is 10 Pa, and the growth time of the two materials is 15 min. After the growth is completed, they are placed in an oven for annealing at a temperature of 250° C. for 4 h. After the annealing is completed, an integrated heating and temperature measurement composite film is obtained;

[0042] f. Preparation of insulating protective layer: Bond the surface of the integrated heating and temperature measuring composite film obtained in step e and lead out the leads, and coat the surface with SiO2 insulating layer 7 as a packaging and protective layer. The RF sputtering vacuum degree is 2×10 -5 Pa, the growth gas pressure is 10Pa, the oxygen and argon contents are 100% respectively, the growth power is 80W, the growth temperature is 500℃, the growth time is 600min, and annealing is carried out in a tubular furnace. The annealing temperature is 600℃, the heating time is 10℃ / min, the holding time is 60min, the cooling time is 10℃ / min, and the annealing atmosphere is oxygen, so as to obtain a thin film integrated temperature control chip material.

[0043] Example 4

[0044] The material composition of the thin film integrated temperature control chip is based on Example 1, and the specific operation is carried out according to the following steps:

[0045] a. Substrate cleaning: ultrasonically clean a 0.5-inch fluorphlogopite substrate 1 using acetone, anhydrous ethanol, deionized water and anhydrous ethanol respectively, with each cleaning time being 30 minutes. After cleaning, the surface of the fluorphlogopite substrate 1 is blown dry with high-purity dry nitrogen;

[0046] b. Preparation of buffer layer: BaZrO3 is selected as the material of the insulating buffer layer 2, and the fluorphlogopite mica substrate 1 obtained in step a is subjected to DC magnetron sputtering for growing the insulating buffer layer 2, and the RF sputtering conditions are: growth pressure of 1 Pa, oxygen and argon contents of 50% respectively, growth power of 50 W, growth temperature of 150° C., growth time of 420 min, and annealing treatment is carried out in a tubular furnace, the annealing temperature is 450° C., the heating time is 5° C. / min, the holding time is 30 min, the cooling time is 5° C. / min, and the annealing atmosphere is nitrogen, so as to obtain the insulating buffer layer 2;

[0047] c. Preparation of heating layer: platinum material is selected as the material of heating film 3, and the fluorphlogopite substrate 1 with insulating buffer layer 2 obtained in step b is used for growing heating film 3 by DC magnetron sputtering, and a mask is used to cover 1 / 3 of the surface of insulating buffer layer 2, and sputtering is carried out on the remaining 2 / 3. The sputtering conditions are: growth pressure is 5Pa, oxygen and argon content are 50% respectively, growth power is 50W, growth temperature is 100°C, growth time is 40min, annealing treatment is carried out in a tubular furnace, annealing temperature is 350°C, heating time is 5°C / min, holding time is 30min, cooling time is 5°C / min, annealing atmosphere is nitrogen, and heating film 3 material is obtained;

[0048] d. Preparation of negative temperature coefficient thermistor film: LaMnO-based material is selected as the material of the thermosensitive film 4, and the heating film 3 material prepared in step c is placed in a magnetron sputtering device for negative temperature coefficient thermistor film growth, and the prepared 2 / 3 part of the heating film 3 is covered with a mask, and then the remaining 1 / 3 part is sputtered, and the sputtering conditions are: growth pressure is 1Pa, oxygen and argon content are 50% respectively, growth power is 50W, growth temperature is 200℃, growth time is 20min, annealing treatment is carried out in a tube furnace, annealing temperature is 850℃, heating time is 8℃ / min, holding time is 30min, cooling time is 8℃ / min, annealing atmosphere is air, and negative temperature coefficient thermistor film 4 material is obtained;

[0049] e. Electrode preparation: The surfaces of the heating film 3 material obtained in step c and the negative temperature coefficient thermistor film 4 obtained in step b are covered with electrode masks respectively, and are placed in the tray of the DC sputtering equipment again to prepare Ni / Au electrodes according to the conventional method. In this process, the heating film 3 material and the negative temperature coefficient thermistor film 4 material are partially covered with electrode masks respectively. The growth power is 40W, the growth pressure is 1Pa, and the growth time of the two materials is 3min and 10min respectively. After the growth is completed, they are placed in an oven for annealing at a temperature of 200°C for 2h. After the annealing is completed, an integrated heating and temperature measurement composite film is obtained;

[0050] f. Preparation of insulating protective layer: Bond the surface of the integrated heating and temperature measuring composite film obtained in step e and lead out the leads, and coat the surface with Si3N4 insulating layer 7 as a packaging and protective layer. The RF sputtering vacuum degree is 5×10 -4 Pa, the growth gas pressure is 1Pa, the oxygen and argon contents are 50% respectively, the growth power is 40W, the growth temperature is 150°C, the growth time is 300min, and annealing is carried out in a tubular furnace, the annealing temperature is 400°C, the heating time is 4°C / min, the holding time is 60min, the cooling time is 4°C / min, and the annealing atmosphere is nitrogen, thereby obtaining a thin film integrated temperature control chip material.

[0051] Example 5

[0052] The material composition of the thin film integrated temperature control chip is based on Example 1, and the specific operation is carried out according to the following steps:

[0053] a. Substrate cleaning: ultrasonically clean the 1-inch aluminum nitride substrate 1 using acetone, anhydrous ethanol, deionized water and anhydrous ethanol respectively, with the cleaning time being 15 minutes each. After cleaning, the surface of the aluminum nitride substrate 1 is blown dry with high-purity dry nitrogen;

[0054] b. Preparation of buffer layer: Al2O3 is selected as the material of the insulating buffer layer 2, and the aluminum nitride substrate 1 obtained in step a is subjected to DC magnetron sputtering for growing the insulating buffer layer 2, and the RF sputtering conditions are: growth pressure of 5 Pa, oxygen and argon contents of 30% respectively, growth power of 60 W, growth temperature of 300°C, and growth time of 200 min. Annealing treatment is carried out in a tubular furnace, the annealing temperature is 500°C, the heating time is 4°C / min, the holding time is 40 min, the cooling time is 4°C / min, and the annealing atmosphere is argon, and the insulating buffer layer 2 is obtained;

[0055] c. Preparation of heating layer: iron-chromium-aluminum alloy is selected as the material of heating film 3, and the substrate 1 with insulating buffer layer 2 obtained in step b is used for growing heating film 3 by DC magnetron sputtering, and a mask is used to cover 1 / 3 of the surface of insulating buffer layer 2, and sputtering is carried out on the remaining 2 / 3. The sputtering conditions are: growth pressure is 5Pa, oxygen and argon content are 30% respectively, growth power is 60W, growth temperature is 300℃, growth time is 80min, annealing treatment is carried out in a tube furnace, annealing temperature is 500℃, heating time is 8℃ / min, holding time is 40min, cooling time is 4℃ / min, annealing atmosphere is argon, and heating film 3 material is obtained;

[0056] d. Preparation of negative temperature coefficient thermistor film: MnCoNiO-based material is selected as the material of the thermosensitive film 4, and the heating film 3 material prepared in step c is placed in a magnetron sputtering device for negative temperature coefficient thermistor film growth, and the prepared 2 / 3 part of the heating film 3 is covered with a mask, and then the remaining 1 / 3 part is sputtered, and the sputtering conditions are: growth pressure is 5Pa, oxygen and argon content are 30% respectively, growth power is 60W, growth temperature is 400℃, growth time is 100min, annealing treatment is carried out in a tube furnace, annealing temperature is 600℃, heating time is 4℃ / min, holding time is 40min, cooling time is 4℃ / min, annealing atmosphere is argon, and negative temperature coefficient thermistor film 4 material is obtained;

[0057] e. Electrode preparation: The surfaces of the heating film 3 material obtained in step c and the negative temperature coefficient thermistor film 4 obtained in step d are covered with electrode masks respectively, and are placed in the tray of the DC sputtering equipment again to prepare Ni / Au electrodes according to the conventional method. In this process, the heating film 3 material and the negative temperature coefficient thermistor film 4 material are partially covered with electrode masks respectively, the growth power is 20W, the growth pressure is 5Pa, and the growth time of the two materials is 8min respectively. After the growth is completed, they are placed in an oven for annealing at a temperature of 230°C for 4h. After the annealing is completed, an integrated heating and temperature measurement composite film is obtained;

[0058] f. Preparation of insulating protective layer: Bond the surface of the integrated heating and temperature measuring composite film obtained in step e and lead out the leads, and coat the surface with Si3N4 insulating layer 7 as a packaging and protective layer. The RF sputtering vacuum degree is 2×10 -3 The growth pressure is 5Pa, the oxygen and argon contents are 30% respectively, the growth power is 60W, the growth temperature is 450℃, the growth time is 400min, and the annealing treatment is carried out in a tubular furnace. The annealing temperature is 350℃, the heating time is 8℃ / min, the holding time is 55min, the cooling time is 8℃ / min, and the annealing atmosphere is argon, so as to obtain a thin film integrated temperature control chip material.

[0059] Example 6

[0060] The material composition of the thin film integrated temperature control chip is based on Example 1, and the specific operation is carried out according to the following steps:

[0061] a. Substrate cleaning: ultrasonically clean the 6-inch alumina substrate 1 using acetone, anhydrous ethanol, deionized water and anhydrous ethanol respectively, with each cleaning time being 25 minutes. After cleaning, the surface of the alumina substrate 1 is blown dry with high-purity dry nitrogen;

[0062] b. Preparation of buffer layer: SiO2 is selected as the material of the insulating buffer layer 2, and the alumina substrate 1 obtained in step a is subjected to DC magnetron sputtering for growing the insulating buffer layer 2, and the RF sputtering conditions are: growth pressure is 2Pa, oxygen and argon contents are 60% respectively, growth power is 70W, growth temperature is 350°C, and growth time is 100min. Annealing treatment is carried out in a tubular furnace, the annealing temperature is 400°C, the heating time is 2°C / min, the holding time is 45min, the cooling time is 2°C / min, and the annealing atmosphere is hydrogen, and the insulating buffer layer 2 is obtained;

[0063] c. Preparation of heating layer: Tantalum nitride is selected as the material of heating film 3, and the substrate 1 with insulating buffer layer 2 obtained in step b is used for growing heating film 3 by DC magnetron sputtering, and 1 / 3 of the surface of insulating buffer layer 2 is covered by mask, and sputtering is carried out on the remaining 2 / 3, and the sputtering conditions are: growth pressure is 2Pa, oxygen and argon content is 60% respectively, growth power is 70W, growth temperature is 350℃, growth time is 110min, annealing treatment is carried out in a tube furnace, annealing temperature is 450℃, heating time is 2℃ / min, holding time is 45min, cooling time is 2℃ / min, annealing atmosphere is hydrogen, and heating film 3 material is obtained;

[0064] d. Preparation of negative temperature coefficient thermistor film: LaMnO-based material is selected as the material of the thermosensitive film 4, and the heating film 3 material prepared in step c is placed in a magnetron sputtering device for negative temperature coefficient thermistor film growth, and the prepared 2 / 3 part of the heating film 3 is covered with a mask, and then the remaining 1 / 3 part is sputtered, and the sputtering conditions are: growth pressure is 2Pa, oxygen and argon content are 60% respectively, growth power is 70W, growth temperature is 450℃, growth time is 110min, annealing treatment is carried out in a tube furnace, annealing temperature is 700℃, heating time is 2℃ / min, holding time is 45min, cooling time is 2℃ / min, annealing atmosphere is hydrogen, and negative temperature coefficient thermistor film 4 material is obtained;

[0065] e. Electrode preparation: The surfaces of the heating film 3 material obtained in step c and the negative temperature coefficient thermistor film 4 obtained in step d are covered with electrode masks respectively, and are placed in the tray of the DC sputtering equipment again to prepare Cr / Au or Ni / Au electrodes according to the conventional method. In this process, the heating film 3 material and the negative temperature coefficient thermistor film 4 material are partially covered with electrode masks respectively, the growth power is 40W, the growth pressure is 2Pa, and the growth time of the two materials is 12min respectively. After the growth is completed, they are placed in an oven for annealing at a temperature of 155°C for 3h. After the annealing is completed, an integrated heating and temperature measurement composite film is obtained;

[0066] f. Preparation of insulating protective layer: Bond the surface of the integrated heating and temperature measuring composite film obtained in step e and lead out the leads, and coat the surface with Al2O3 insulating layer 7 as a packaging and protective layer. The RF sputtering vacuum degree is 2×10 -3 Pa, the growth gas pressure is 2Pa, the oxygen and argon contents are 60% respectively, the growth power is 70W, the growth temperature is 350℃, the growth time is 550min, and annealing is carried out in a tubular furnace. The annealing temperature is 350℃, the heating time is 2℃ / min, the holding time is 55min, the cooling time is 2℃ / min, and the annealing atmosphere is hydrogen, so as to obtain a thin film integrated temperature control chip material.

[0067] Example 7

[0068] The material composition of the thin film integrated temperature control chip is based on Example 1, and the specific operation is carried out according to the following steps:

[0069] a. Substrate cleaning: ultrasonically clean a 0.8-inch fluorphlogopite substrate 1 using acetone, anhydrous ethanol, deionized water and anhydrous ethanol respectively, with each cleaning time being 30 minutes. After cleaning, the surface of the fluorphlogopite substrate 1 is blown dry with high-purity dry nitrogen;

[0070] b. Preparation of buffer layer: Si3N4 is selected as the material of the insulating buffer layer 2, and the fluorphlogopite substrate 1 obtained in step a is subjected to DC magnetron sputtering for growing the insulating buffer layer 2, and the RF sputtering conditions are: growth pressure of 7Pa, oxygen and argon contents of 25% respectively, growth power of 25W, growth temperature of 350°C, growth time of 600min, and annealing treatment is carried out in a tubular furnace, the annealing temperature is 300°C, the heating time is 10°C / min, the holding time is 60min, the cooling time is 10°C / min, and the annealing atmosphere is argon, and the insulating buffer layer 2 is obtained;

[0071] c. Preparation of heating layer: copper-nickel alloy is selected as the material of heating film 3, and the fluorphlogopite substrate 1 with insulating buffer layer 2 obtained in step b is used for growing heating film 3 by DC magnetron sputtering, and a mask is used to cover 1 / 3 of the surface of insulating buffer layer 2, and sputtering is carried out on the remaining 2 / 3. The sputtering conditions are: growth pressure is 7Pa, oxygen and argon content are 25% respectively, growth power is 25W, growth temperature is 350°C, growth time is 20min, annealing treatment is carried out in a tube furnace, annealing temperature is 300°C, heating time is 10°C / min, holding time is 60min, cooling time is 10°C / min, annealing atmosphere is argon, and heating layer material 2 is obtained;

[0072] d. Preparation of negative temperature coefficient thermistor film: MnCoNiO-based material is selected as the material of the thermosensitive film 4, and the heating film 3 material prepared in step c is placed in a magnetron sputtering device for negative temperature coefficient thermistor film growth, and the prepared 2 / 3 part of the heating film 3 is covered with a mask, and then the remaining 1 / 3 part is sputtered, and the sputtering conditions are: growth pressure is 7Pa, oxygen and argon content are 25% respectively, growth power is 25W, growth temperature is 350℃, growth time is 20min, annealing treatment is carried out in a tube furnace, annealing temperature is 600℃, heating time is 10℃ / min, holding time is 60min, cooling time is 10℃ / min, annealing atmosphere is argon, and negative temperature coefficient thermistor film 4 material is obtained;

[0073] e. Electrode preparation: The surfaces of the heating film 3 material obtained in step c and the negative temperature coefficient thermistor film 4 obtained in step d are covered with electrode masks respectively, and are placed in the tray of the DC sputtering equipment again to prepare Cr / Au or Ni / Au electrodes according to the conventional method. In this process, the heating film 3 material and the negative temperature coefficient thermistor film 4 material are partially covered with electrode masks respectively, the growth power is 25W, the growth pressure is 7Pa, and the growth time of the two materials is 15min respectively. After the growth is completed, they are placed in an oven for annealing at a temperature of 200°C for 4h. After the annealing is completed, an integrated heating and temperature measurement composite film is obtained;

[0074] f. Preparation of insulating protective layer: Bond the surface of the integrated heating and temperature measuring composite film obtained in step e and lead out the leads, and coat the surface with AlN insulating layer 7 as a packaging and protective layer. The RF sputtering vacuum degree is 2×10 -3 Pa, the growth gas pressure is 7Pa, the oxygen and argon contents are 25% respectively, the growth power is 25W, the growth temperature is 350°C, the growth time is 600min, and annealing is carried out in a tubular furnace, the annealing temperature is 300°C, the heating time is 10°C / min, the holding time is 60min, the cooling time is 10°C / min, and the annealing atmosphere is argon, thereby obtaining a thin film integrated temperature control chip material.

[0075] Example 8

[0076] The material composition of the thin film integrated temperature control chip is based on Example 1, and the specific operation is carried out according to the following steps:

[0077] a. Substrate cleaning: A 3-inch aluminum oxide substrate 1 was ultrasonically cleaned using acetone, anhydrous ethanol, deionized water and anhydrous ethanol respectively, with each cleaning time being 10 minutes. After cleaning, the surface of the substrate 1 was blown dry with high-purity dry nitrogen;

[0078] b. Preparation of buffer layer: AlN is selected as the material of the insulating buffer layer 2, and the alumina substrate 1 obtained in step a is subjected to DC magnetron sputtering for growing the insulating buffer layer 2, and the RF sputtering conditions are: growth pressure of 4 Pa, oxygen and argon contents of 75% respectively, growth power of 55 W, growth temperature of 50° C., and growth time of 60 min. Annealing treatment is carried out in a tubular furnace, the annealing temperature is 600° C., the heating time is 1° C. / min, the holding time is 10 min, the cooling time is 1-10° C. / min, and the annealing atmosphere is air, thus obtaining the insulating buffer layer 2;

[0079] c. Preparation of heating layer: iron-chromium-aluminum alloy is selected as the material of heating film 3, and the substrate 1 with insulating buffer layer 2 obtained in step b is used for growing heating film 3 by DC magnetron sputtering, and a mask is used to cover 1 / 3 of the surface of insulating buffer layer 2, and sputtering is carried out on the remaining 2 / 3. The sputtering conditions are: growth pressure is 4Pa, oxygen and argon content is 75% respectively, growth power is 55W, growth temperature is 50°C, growth time is 20min, annealing treatment is carried out in a tube furnace, annealing temperature is 600°C, heating time is 1°C / min, holding time is 10min, cooling time is 1°C / min, annealing atmosphere is air, and heating film 3 material is obtained;

[0080] d. Preparation of negative temperature coefficient thermistor film: LaMnO-based material is selected as the material of the thermosensitive film 4, and the heating film 3 material prepared in step c is placed in a magnetron sputtering device for negative temperature coefficient thermistor film growth, and the prepared 2 / 3 part of the heating film 3 is covered with a mask, and then the remaining 1 / 3 part is sputtered, and the sputtering conditions are: growth pressure is 4Pa, oxygen and argon content are 75% respectively, growth power is 55W, growth temperature is 50°C, growth time is 20min, annealing treatment is carried out in a tube furnace, annealing temperature is 1000°C, heating time is 1°C / min, holding time is 10min, cooling time is 1°C / min, annealing atmosphere is air, and negative temperature coefficient thermistor film 4 material is obtained;

[0081] e. Electrode preparation: The surfaces of the heating film 3 material obtained in step c and the negative temperature coefficient thermistor film 4 obtained in step d are covered with electrode masks respectively, and are placed in the tray of the DC sputtering equipment again to prepare Ni / Au electrodes according to the conventional method. In this process, the heating film 3 material and the negative temperature coefficient thermistor film 4 material are partially covered with electrode masks respectively, the growth power is 10W, the growth pressure is 4Pa, and the growth time of the two materials is 12min respectively. After the growth is completed, they are placed in an oven for annealing at a temperature of 175°C for 1h. After the annealing is completed, an integrated heating and temperature measurement composite film is obtained;

[0082] f. Preparation of insulating protective layer: Bond the surface of the integrated heating and temperature measuring composite film obtained in step e to the lead wire, and coat the surface with a SiO2 insulating layer (7) as a packaging and protective layer. The RF sputtering vacuum is 2×10 -5 Pa, the growth gas pressure is 4Pa, the oxygen and argon contents are 75% respectively, the growth power is 55W, the growth temperature is 50°C, the growth time is 60min, and annealing is carried out in a tubular furnace, the annealing temperature is 600°C, the heating time is 1°C / min, the holding time is 10min, the cooling time is 1°C / min, and the annealing atmosphere is air, so as to obtain a thin film integrated temperature control chip material.

[0083] Example 9

[0084] The thin film integrated temperature control chip prepared in Example 1 was tested and applied;

[0085] A constant temperature oil bath was used as the constant temperature device, and the temperature was tested by a computer-controlled thermometer. The temperature control range was 273.15-353.15K, the temperature increase was 5K each time, and the constant temperature time was 45min per 5K. The resistance-temperature relationship test data obtained are shown in Table 1.

[0086] Table 1

[0087] Temperature / K Resistance / kΩ Temperature / K Resistance / kΩ 273.15 480.532 313.15 95.363 278.15 383.971 318.15 79.899 283.15 308.980 323.15 67.278 288.15 250.309 328.15 56.925 293.15 204.077 333.15 48.389 298.15 167.394 338.15 41.316 303.15 138.007 343.15 35.428 308.15 114.413 348.15 30.504

[0088] The resistance-temperature performance relationship was obtained according to Table 1. Figure 3 As shown in Table 1 and Figure 3 It can be seen that the resistance-temperature performance curve of the prepared thin-film integrated temperature control chip shows a downward trend as the temperature rises, which conforms to the negative temperature coefficient relationship.

Claims

1. A thin film integrated temperature control chip material, characterized in that The chip comprises a substrate (1), an insulating buffer layer (2), a heating film (3), a thermosensitive film (4), interdigital electrodes (5), terminal electrodes (6) and an insulating layer (7). An insulating buffer layer (2), a heating film (3), a thermosensitive film (4), interdigital electrodes (5) and terminal electrodes (6) are provided between the substrate (1) and the insulating layer (7). The thermosensitive film (4) is provided on one side of the surface of the insulating buffer layer (2) and the heating film (3) is provided on the other side. Terminal electrodes (6) are provided at both ends of the surface of the heating film (3), and the interdigital electrodes (5) are provided on the surface of the thermosensitive film (4). The specific operation is performed according to the following steps: a. Substrate cleaning: ultrasonically cleaning the substrate (1) with acetone, anhydrous ethanol, deionized water and anhydrous ethanol respectively, with the cleaning time being 10-30 minutes respectively, and blowing the surface of the substrate (1) dry with high-purity dry nitrogen after cleaning, wherein the substrate (1) is silicon oxide, silicon nitride, aluminum oxide, aluminum nitride, alloy material or fluorphlogopite, and the substrate size is 0.1-6 inches; b. Preparation of buffer layer: SrTiO3, BaTiO3, SrZrO3, BaZrO3, Al2O3, AlN, SiO2 or Si3N4 are selected as the insulating buffer layer (2) material, and the substrate (1) obtained in step a is grown with DC magnetron sputtering. The RF sputtering conditions are: the growth pressure is 10 -1 -10Pa, oxygen and argon contents are 0%-100% respectively, growth power is 10-80W, growth temperature is 50-500°C, growth time is 60-600min, annealing treatment is carried out in a tube furnace, annealing temperature is 300-600°C, heating time is 1-10°C / min, holding time is 10-60min, cooling time is 1-10°C / min, annealing atmosphere is air, oxygen, nitrogen, argon or hydrogen, thus obtaining an insulating buffer layer (2); c. Preparation of the heating layer: Tantalum nitride, copper-nickel alloy, nickel-chromium alloy, iron-chromium-aluminum alloy, or platinum material is selected as the material of the heating film (3). The substrate (1) with the insulating buffer layer (2) obtained in step b is used for growing the heating film (3) by direct current magnetron sputtering. A mask is used to cover 1 / 3 of the surface of the insulating buffer layer (2), and sputtering is carried out on the remaining 2 / 3. The sputtering conditions are: the growth gas pressure is 10 -1 -10Pa, oxygen and argon contents are 0%-100% respectively, growth power is 10-80W, growth temperature is 50-500℃, growth time is 20-120min, annealing treatment is carried out in a tube furnace, annealing temperature is 300-600℃, heating time is 1-10℃ / min, holding time is 10-60min, cooling time is 1-10℃ / min, annealing atmosphere is air, oxygen, nitrogen, argon or hydrogen, and a heated film (3) material is obtained; d. Preparation of negative temperature coefficient thermistor film: MnCoNiO or LaMnO materials are selected as the thermosensitive film (4) material, the heating film (3) material prepared in step c is placed in a magnetron sputtering device to grow a negative temperature coefficient thermistor film, 2 / 3 of the prepared heating film (3) is covered with a mask, and the remaining 1 / 3 is sputtered. The sputtering conditions are: the growth pressure is 10 -1 -10Pa, oxygen and argon contents are 0%-100% respectively, growth power is 10-80W, growth temperature is 50-500℃, growth time is 20-120min, annealing treatment is carried out in a tube furnace, annealing temperature is 300-1000℃, heating time is 1-10℃ / min, holding time is 10-60min, cooling time is 1-10℃ / min, annealing atmosphere is air, oxygen, nitrogen, argon or hydrogen, and negative temperature coefficient thermistor film (4) material is obtained; e. Electrode preparation: The heating film (3) material obtained in step c and the negative temperature coefficient thermistor (4) layer obtained in step d are covered with electrode masks respectively, and are placed in the tray of the DC sputtering device again to prepare Cr / Au or Ni / Au electrodes according to the conventional method. In this process, the heating film (3) material and the negative temperature coefficient thermistor (4) material are covered with electrode masks respectively, and the growth power is 10-50W and the growth pressure is 10 -1 -10Pa, the growth time of the two materials is 3-15min respectively, after the growth is completed, they are placed in an oven for annealing at a temperature of 125-250℃ for 1-4 h, after the annealing is completed, an integrated heating and temperature measurement composite film is obtained; f. Preparation of insulating protective layer: Bond the surface of the integrated heating and temperature measuring composite film obtained in step e to the lead wire, and coat the surface with an insulating layer (7) as a packaging and protective layer. Al2O3, AlN, SiO2 or Si3N4 are selected as the insulating layer (7) material. The RF sputtering vacuum degree is 2×10 -3 -2×10 -5 Pa, the growth pressure is 10 -1 -10Pa, oxygen and argon content are 0%-100% respectively, growth power is 10-80W, growth temperature is 50-500℃, growth time is 60-600min, annealing treatment is carried out in a tubular furnace, annealing temperature is 300-600℃, heating time is 1-10℃ / min, holding time is 10-60min, cooling time is 1-10℃ / min, annealing atmosphere is air, oxygen, nitrogen, argon or hydrogen, and a thin film integrated temperature control chip material is obtained.

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