NL2032876B1 - Method for preparing thermosensitive thin film with heat insulation buffer layer structure - Google Patents

Method for preparing thermosensitive thin film with heat insulation buffer layer structure Download PDF

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Publication number
NL2032876B1
NL2032876B1 NL2032876A NL2032876A NL2032876B1 NL 2032876 B1 NL2032876 B1 NL 2032876B1 NL 2032876 A NL2032876 A NL 2032876A NL 2032876 A NL2032876 A NL 2032876A NL 2032876 B1 NL2032876 B1 NL 2032876B1
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Prior art keywords
silicon
thin film
silicon substrate
buffer layer
heat insulation
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NL2032876A
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Dutch (nl)
Inventor
Wang Zhenhua
Chang Aimin
Pan Ye
Yang Bo
Kong Wenwen
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Zhongke Sensor Foshan Tech Co Ltd
Xinjiang Technical Inst Of Physics And Chemistry Chinese Academy Of Sciences
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Publication of NL2032876B1 publication Critical patent/NL2032876B1/en

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C17/00Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/075Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thin film techniques
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C7/00Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
    • H01C7/006Thin film resistors
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C7/00Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
    • H01C7/008Thermistors

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  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Thermistors And Varistors (AREA)

Abstract

The present invention discloses a method for preparing a thermosensitive thin film. with a heat insulation buffer layer structure. The method includes: preparing a heat insulation buffer layer on a surface of a silicon substrate; preparing a silicon dioxide insulation layer on a surface of the heat insulation buffer layer; and preparing a thermosensitive thin film. on a surface of the silicon dioxide insulation layer, thus obtaining the thermosensitive thin film. with the heat insulation buffer layer structure. The heat insulation buffer layer is formed into a porous silicon—based structure with different structural characteristics by growing silicon columns, silicon balls or silicon rods; a heat insulation effect between the thermosensitive thin film and the silicon substrate is achieved using air stored inside pores, so that the overall thermal capacity and heat dissipation of the thermosensitive thin film are reduced.

Description

P1540 /NLpd
METHOD FOR PREPARING THERMOSENSITIVE THIN FILM WITH HEAT
INSULATION BUFFER LAYER STRUCTURE
TECHNICAL FIELD
The present invention relates to a method for preparing a thermosensitive thin film with a heat insulation buffer layer structure.
BACKGROUND ART
A negative temperature coefficient (NTC) thermistor is a com- mon temperature measurement and control element with the charac- teristics of high temperature measurement accuracy, high sensitiv- ity, good reliability, low cost, long service life and the like.
It is widely used in aviation, marine and civil fields. With the continuous advancement of the electronic industry and the level of an information technology, a modern electronic information system is developing towards miniaturization and monolithic integration.
Compared with a bulk ceramic thermistor, a thin-film NTC thermis- tor more easily achieves objectives of miniaturization, fast re- sponse and integration of temperature sensors, and has a wide ap- plication prospect in the fields of semiconductors, integrated circuits, and micro-nano devices.
Since a thermosensitive thin film is a material relying on a substrate, its structure and characteristics are inevitably af- fected by the substrate. At present, selection of a substrate ma- terial for the thermosensitive thin film is mainly based on three aspects: 1. The thermal expansion coefficient of the substrate should be close to that of the thermosensitive thin film, so that the problem of cracking of the thin film during thermal treatment and thermal environment application can be effectively avoided. 2.
The lattice match degree between the substrate and the material is high, so that it is expected to prepare a high-quality single- crystal epitaxial thin film. 3. The substrate is suitable for a modern semiconductor micro-machining technology, which is condu- cive to the instrumentation and integration of thin films.
Among the above-mentioned various substrate materials, a Si- based substrate has been applied in other passive sensitive thin- film sensors such as magnetoresistive and magnetic sensors due to its advantages of easy integration and low price, and is the most promising substrate material for achieving the application of the thermosensitive thin films. In the process of transitioning from basic research on thermosensitive thin films to practical use of thin-film temperature sensors, in addition to achieving Si-based hetero-growth of a high-quality film with a uniform thickness, the influence of a substrate material on a thermal conduction process of a thin film also needs to be considered. If a thermosensitive thin film is directly deposited on a surface of an ordinary Si substrate, the high thermal conductivity (156W/cm-°C) of the Si substrate will cause heat conduction between the thermosensitive thin film and the substrate, which will imperceptibly increase the thermal capacity of a sensitive unit and prolong the response time of the thin film material. Therefore, it is difficult to meet the demand for fast response and sensing to temperatures in the field of extreme temperature monitoring.
In order to avoid the above problems, the present invention designs a heat insulation layer structure on a surface of a sili- con substrate to ensure that a silicon substrate thermosensitive thin film makes a quick dynamic response to temperatures.
SUMMARY
The present invention aims to provide a method for preparing a thermosensitive thin film with a heat insulation buffer layer structure. The method includes: first preparing a heat insulation buffer layer on a surface of a silicon substrate; preparing a sil- icon dioxide insulation layer on a surface of the heat insulation buffer layer; and finally preparing a thermosensitive thin film on a surface of the silicon dioxide insulation layer, thus obtaining the thermosensitive thin film with the heat insulation buffer lay- er structure. The heat insulation buffer layer is formed into a porous silicon-based structure with different structural charac- teristics by growing silicon columns, silicon balls or silicon rods; a heat insulation effect between the thermosensitive thin film and the silicon substrate is achieved using air stored inside pores, so that the overall thermal capacity and heat dissipation of the thermosensitive thin film are reduced; the response time of a thermistor is shortened; and the thermosensitive thin film is extremely applicable to the field of fast-response temperature monitoring. The thermosensitive thin film with the heat insulation buffer layer structure obtained by the method of the present in- vention solves the key technical problem in a process of transi- tioning of a thermosensitive thin film from basic research to practical use research. The method is easy to achieve, good in re- petitiveness, easy to operate and applicable to various thermosen- sitive thin films, and is general to development of all types of thermosensitive thin films.
The present invention discloses a method for preparing a thermosensitive thin film with a heat insulation buffer layer structure. The method is carried out according to the following steps: a. preparation of a heat insulation buffer layer: first im- mersing a purchased silicon substrate (1) in acetone, absolute ethanol and deionized water in sequence for ultrasonic washing for three times, each washing time being 5-10 min; taking out the sil- icon substrate (1); blowing a surface of the silicon substrate (1) to dry with high-purity nitrogen; manufacturing masks with various shapes on the surface of the silicon substrate (1), and putting the silicon substrate (1) into a cavity of electron beam evapora- tion equipment; growing silicon materials (2) at hollow parts of the masks on the surface of the silicon substrate (1) to form sil- icon columns, silicon balls or silicon rods; controlling heights of the silicon materials (2) of the silicon columns, silicon balls or silicon rods to be 10 nm to 200 um by means of adjusting a voltage to 1-2 kV and evaporation time to 5-60 min; and achieving heat insulation using air stored in holes (3) at gaps between the silicon columns, silicon balls or silicon rods; b. preparation of a silicon dioxide insulation layer: putting the silicon substrate (1) prepared in the step a into a thermal oxidation furnace for thermal oxidization at a temperature of 500- 1,050°C and an oxygen pressure of 10°-10° Pa for 30-120 min, thus obtaining the silicon dioxide insulation layer (4) with a growth thickness of 100-500 nm; c. preparation of a thermosensitive thin film: preparing a thermosensitive thin film material on the surface of the silicon substrate (1) obtained in the step b by using a magnetron sputter- ing or pulsed laser deposition or ion beam evaporation physical deposition method, wherein the thermosensitive thin film material is a vanadium oxide or Mn-Co-Ni-based negative temperature coeffi- cient (NTC) thermistor material (5).
According to the method for preparing a thermosensitive thin film with a heat insulation buffer layer structure, the thermosen- sitive thin film with the heat insulation buffer layer structure obtained by the method of the present invention solves the key technical problem in a process of transitioning of a thermosensi- tive thin film from basic research to practical use research. The method is applicable to various thermosensitive thin films, and is general to development of all types of thermosensitive thin films.
The thermosensitive thin film can be developed into a micro ther- mosensitive resistor with a fast response characteristic.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic structural diagram of a thermosensitive thin film with a heat insulation buffer layer structure of the present invention.
FIG. 2 is an X-Ray Diffraction (XRD) spectrum of a thermosen- sitive thin film material with a heat insulation buffer layer structure.
FIG. 3 is an Atomic Force Microscope (AFM) diagram of a ther- mosensitive thin film material with a heat insulation buffer layer structure.
FIG. 4 is a resistance-temperature relationship diagram of a thermosensitive thin film element with a heat insulation buffer layer structure.
FIG. 5 shows response time of a thermosensitive thin film el- ement with a heat insulation buffer layer structure.
DETAILED DESCRIPTION OF THE EMBODIMENTS
Embodiment 1 a. Preparation of a heat insulation buffer layer: a purchased gilicon substrate 1 is first immersed in acetone, absolute ethanol 5 and deionized water in sequence for ultrasonic washing for three times, each washing time being 5 min; the silicon substrate 1 is taken out; a surface of the silicon substrate 1 is blown to dry with high-purity nitrogen; masks with various shapes are manufac- tured on the surface of the silicon substrate 1, and the silicon substrate 1 is put into a cavity of electron beam evaporation equipment; silicon materials 2 are grown at hollow parts of the masks on the surface of the silicon substrate 1 to form silicon columns; heights of the silicon materials 2 of the silicon columns are controlled to be 10 nm by means of adjusting a voltage to 1 kV and evaporation time to 5 min; and heat insulation is achieved by using air stored in holes 3 at gaps between the silicon columns. b. Preparation of a silicon dioxide insulation layer: the silicon substrate 1 prepared in the step a is put into a thermal oxidation furnace for thermal oxidization at a temperature of 500°C and an oxygen pressure of 10° Pa for 30 min, thus obtaining the silicon dioxide insulation layer 4 with a growth thickness of 100 nm. c. Preparation of a thermosensitive thin film: a thermosensi- tive thin film material is prepared on the surface of the silicon substrate 1 obtained in the step b by using a magnetron sputtering method, wherein the thermosensitive thin film material is a vana- dium oxide NTC thermistor material 5.
Embodiment 2 a. Preparation of a heat insulation buffer layer: a purchased silicon substrate 1 is first immersed in acetone, absolute ethanol and deionized water in sequence for ultrasonic washing for three times, each washing time being 10 min; the silicon substrate 1 is taken out; a surface of the silicon substrate 1 is blown to dry with high-purity nitrogen; masks with various shapes are manufac- tured on the surface of the silicon substrate 1, and the silicon substrate 1 is put into a cavity of electron beam evaporation equipment; silicon materials 2 are grown at hollow parts of the masks on the surface of the silicon substrate 1 to form silicon balls; heights of the silicon materials 2 of the silicon balls are controlled to be 200 um by means of adjusting a voltage to 2 kV and evaporation time to 60 min; and heat insulation is achieved by using air stored in holes 3 at gaps between the silicon balls. b. Preparation of a silicon dioxide insulation layer: the silicon substrate 1 prepared in the step a is put into a thermal oxidation furnace for thermal oxidization at a temperature of 1,050°C and an oxygen pressure of 10° Pa for 120 min, thus obtain- ing the silicon dioxide insulation layer 4 with a growth thickness of 500 nm. c. Preparation of a thermosensitive thin film: a thermosensi- tive thin film material is prepared on the surface of the silicon substrate 1 obtained in the step b by using a pulse laser deposi- tion method, wherein the thermosensitive thin film material is a
Mn-Co-Ni NTC thermistor material 5.
Embodiment 3 a. Preparation of a heat insulation buffer layer: a purchased silicon substrate 1 is first immersed in acetone, absolute ethanol and deionized water in sequence for ultrasonic washing for three times, each washing time being 8 min; the silicon substrate 1 is taken out; a surface of the silicon substrate 1 is blown to dry with high-purity nitrogen; masks with various shapes are manufac- tured on the surface of the silicon substrate 1, and the silicon substrate 1 is put into a cavity of electron beam evaporation equipment; silicon materials 2 are grown at hollow parts of the masks on the surface of the silicon substrate 1 to form silicon rods; heights of the silicon materials 2 of the silicon rods are controlled to be 150 um by means of adjusting a voltage to 1.5 kV and evaporation time to 20 min; and heat insulation is achieved by using air stored in holes 3 at gaps between the silicon rods. b. Preparation of a silicon dioxide insulation layer: the silicon substrate 1 prepared in the step a is put into a thermal oxidation furnace for thermal oxidization at a temperature of 1,000°C and an oxygen pressure of 10% Pa for 100 min, thus obtain- ing the silicon dioxide insulation layer 4 with a growth thickness of 300 nm.
c. Preparation of a thermosensitive thin film: a thermosensi- tive thin film material is prepared on the surface of the silicon substrate 1 obtained in the step b by using a ion beam evaporation physical deposition method, wherein the thermosensitive thin film material is a vanadium oxide NTC thermistor material 5.
Embodiment 4
An XRD test shown in FIG. 2, an AFM test shown in FIG. 3, an electric property test shown in FIG. 4 and a response time test shown in FIG. 5 are carried out on any thermosensitive thin film material with the heat insulation buffer layer structure obtained in Embodiments 1-3. Results are as shown in the figures. It can be seen from the figures that the response time of the thin film with the heat insulation buffer layer structure is shorter than the re- sponse time of a thermosensitive thin film on the surface of an ordinary silicon substrate.

Claims (1)

CONCLUSIESCONCLUSIONS 1. Werkwijze voor het vervaardigen van een warmtegevoelige dunne film met een warmte-isolerende bufferlaagstructuur, met het ken- merk, dat de werkwijze wordt uitgevoerd in overeenstemming met de volgende stappen:1. Method for manufacturing a heat-sensitive thin film with a heat-insulating buffer layer structure, characterized in that the method is carried out in accordance with the following steps: a. bereiding van een warmte-isolerende bufferlaag: eerst een aan- gekocht siliciumsubstraat (1) achtereenvolgens onderdompelen in aceton, absolute ethanol en gedeïoniseerd water voor ultrasoon wassen gedurende drie keer, waarbij elke wastijd 5 tot 10 min is; het uitnemen van het siliciumsubstraat (1); het blazen van een op- pervlak van het siliciumsubstraat (1) om te drogen met stikstof van hoge zuiverheid; het vervaardigen van maskers met verschillen- de vormen op het oppervlak van het siliciumsubstraat (1), en het plaatsen van het siliciumsubstraat (1) in een holte van elektro- nenstraalverdampingsapparatuur; het groeien van siliciummaterialen (2) op holle delen van de maskers op het oppervlak van het silici- umsubstraat (1) om siliciumkolommen, siliciumballen of silicium- staven te vormen; het regelen van hoogten van de siliciummateria- len (2) van de siliciumkolommen, siliciumballen of siliciumstaven op 10 nm tot 200 pm door middel van het instellen van een spanning op 1 tot 2 kV en verdampingstijd op 5 tot 60 min; en het bereiken van warmte-isolatie met gebruikmaking van lucht die is opgeslagen in gaten (3) bij openingen tussen de siliciumkolommen, silicium- ballen of siliciumstaven;a. Preparation of a heat-insulating buffer layer: first immerse a purchased silicon substrate (1) successively in acetone, absolute ethanol and deionized water for ultrasonic washing for three times, each washing time being 5 to 10 minutes; removing the silicon substrate (1); blowing a surface of the silicon substrate (1) to dry with high purity nitrogen; manufacturing masks of different shapes on the surface of the silicon substrate (1), and placing the silicon substrate (1) in a cavity of electron beam evaporation equipment; growing silicon materials (2) on hollow portions of the masks on the surface of the silicon substrate (1) to form silicon columns, silicon balls or silicon rods; controlling heights of the silicon materials (2) of the silicon columns, silicon balls or silicon rods to 10 nm to 200 pm by setting a voltage to 1 to 2 kV and evaporation time to 5 to 60 min; and achieving thermal insulation using air stored in holes (3) at gaps between the silicon columns, silicon balls or silicon rods; b. bereiding van een siliciumdioxide-isolatielaag: het in stap a bereide siliciumsubstraat (1) in een thermische oxidatieoven plaatsen voor thermische oxidatie bij een temperatuur van 500 totb. preparation of a silicon dioxide insulation layer: placing the silicon substrate (1) prepared in step a into a thermal oxidation furnace for thermal oxidation at a temperature of 500 to 1.050 °C en een zuurstofdruk van 10° tot 10° Pa gedurende 30 tot 120 min waardoor de siliciumdioxide-isolatielaag (4) wordt verkregen met een groeidikte van 100 tot 500 nm;1,050 °C and an oxygen pressure of 10° to 10° Pa for 30 to 120 min, yielding the silicon dioxide insulating layer (4) with a growth thickness of 100 to 500 nm; c. bereiding van een warmtegevoelige dunne film: het bereiden van een warmtegevoelig dunne film-materiaal op het oppervlak van het siliciumsubstraat (1) dat is verkregen in stap b door gebruik te maken van een fysische depositiemethode met magnetronverstuiving of gepulseerde laserdepositie of ionenbundelverdamping, waarbij het warmtegevoelige dunne filmmateriaal een vanadiumoxide of op Mn-Co-Ni gebaseerd thermistormateriaal (5) met negatieve tempera- tuurcoëfficiënt (NTC) is.c. preparation of a heat-sensitive thin film: preparing a heat-sensitive thin film material on the surface of the silicon substrate (1) obtained in step b by using a physical deposition method with microwave sputtering or pulsed laser deposition or ion beam evaporation, wherein the heat-sensitive thin film material is a vanadium oxide or Mn-Co-Ni based thermistor material (5) with negative temperature coefficient (NTC).
NL2032876A 2022-08-29 2022-08-29 Method for preparing thermosensitive thin film with heat insulation buffer layer structure NL2032876B1 (en)

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