CN104003724A - Manufacturing method for oriented thermosensitive thin-film resistor - Google Patents
Manufacturing method for oriented thermosensitive thin-film resistor Download PDFInfo
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- CN104003724A CN104003724A CN201410260345.0A CN201410260345A CN104003724A CN 104003724 A CN104003724 A CN 104003724A CN 201410260345 A CN201410260345 A CN 201410260345A CN 104003724 A CN104003724 A CN 104003724A
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Abstract
The invention relates to a manufacturing method for an oriented thermosensitive thin-film resistor. According to the manufacturing method, lanthanum nitrate, manganese acetate and aluminum nitrate serve as raw materials and are respectively dissolved in glacial acetic acid and ethylene glycol monomethyl ether to obtain a clear solution, the solution is deposited on a (100) oriented lanthanum nickelate substrate through a spin-coating method, volatilized organic matter is pretreated, the needed film thickness is achieved through repeated spin coating, an oriented thermosensitive thin film is obtained through final heat treatment, and the thermosensitive resistor is obtained through manufacturing electrodes. Because the oriented thin film has higher crystal particle ordered arrangement compared with a common thin film, not only can requirements for microminiaturization, integration and utilization in a high-temperature environment of an electronic equipment structure be met, but also the requirement for rapider response of the device in actual application can be met.
Description
Technical field
The preparation method who the present invention relates to a kind of orientation thermosensitive film with fast-response, belongs to technical field of electronic materials.
Background technology
For meeting control, the measurement of electrical equipment under hot conditions, pyrostat is had higher requirement.Conventional temperature sensor is generally with AB
2o
4spinel structure is main negative tempperature coefficient thermistor, and due to the poor great use of device in hot environment that limited of its aging resistance.Perovskite structure ABO
3thermistor because of its at high temperature stable performance, become the type material system of high-temperature thermistor research.Lanthanum manganate base (LaMnO
3) as a kind of typical perovskite structural material, there is good NTC characteristic, and Al doping is a kind of means that effectively improve material constant (B value), so Al doping LaMnO
3thermistor, has great importance as producing high-temperature thermistor.
Film can meet electronic devices and components miniaturization, integrated demand for development, and therefore, in the research field of thermistor, thin-film thermistor has been subject to attention more.And oriented film is due to the orientations of inner crystal grain, exists pole axis, and can have a huge impact many electric properties of material.Therefore in the preparation of thermosensitive material film, control orientation, have great importance for improving its performance.And be orientated thermosensitive film by preparation in this research, for the temperature-sensitive device development of faster response provides support.
Summary of the invention
The object of the invention is, a kind of preparation method who is orientated thermosensitive film resistance is provided, the method is raw material by lanthanum nitrate, manganous acetate and aluminum nitrate, be dissolved in respectively in Glacial acetic acid and ethylene glycol monomethyl ether, obtain pure clear solution, be deposited on by spin-coating method on the nickel acid lanthanum substrate of (100) orientation, pre-treatment volatile organic compounds, repeatedly repeat spin coating and obtain required film thickness, through final thermal treatment, obtain being orientated thermosensitive film.Because the relatively general film of oriented film has higher crystal grain ordered arrangement, not only can meet electronic devices structure microminiaturization, the requirement that integrated and hot environment is used, and can meet in actual applications the demand of the faster response of device.
A kind of preparation method who is orientated thermosensitive film resistance of the present invention, follows these steps to carry out:
A, lanthanum nitrate, manganous acetate and aluminum nitrate are made to raw material, be dissolved in respectively in Glacial acetic acid and ethylene glycol monomethyl ether, wherein the volume ratio of Glacial acetic acid and ethylene glycol monomethyl ether is 1:1, then, at temperature 60-90 DEG C, stirs, to be dissolved complete, stops heating, is cooled to room temperature;
B, three kinds of solution in step a are mixed again, continue to stir 6h, being modulated into concentration is 0.05-0.2mol/L solution, filters, and leaves standstill 8h, forms manganese lanthanum aluminate colloidal sol;
C, utilize spin-coating method, under room temperature, step b manganese lanthanum aluminate colloidal sol is dropped in the nickel acid lanthanum substrate of (100) orientation, even glue 20s on sol evenning machine, rotating speed is 3500r/min, then in tube furnace, keep 3min, treatment temp is 300 DEG C, the organism in volatilization film, repeat even glue masking, obtain the film of 150-1500nm thickness;
D, the film that step c is obtained leave standstill and process 1h at 750 DEG C of temperature, are orientated uniformly thermosensitive film, and then sputter gold electrode on ion sputtering instrument leaves standstill 10min at 200 DEG C of temperature, then welds Pt lead-in wire, can obtain thin-film thermistor.
Step a Raw lanthanum nitrate, manganous acetate and aluminum nitrate be La:Mn:Al=1:0.4-0.7:0.3-0.6 in molar ratio.
A kind of preparation method who is orientated thermosensitive film resistance of the present invention, compared with prior art, the thermistor of gained of the present invention can have the faster response time, can meet in electronic industry production, in structure design, be more convenient for microminiaturized, integrated, the high-temperature behavior that thermistor is good, to having important purposes at the control of the electrical equipment of operation under hot environment, thermometric.
(100) mentioned in the present invention, are technical term speech, refer to the XRD diffraction peak of material thing phase.
Brief description of the drawings
Fig. 1 is the XRD diffracting spectrum of the invention process 1 gained orientation thermosensitive film resistance, has (100) perfectly oriented structure, wherein
for substrate diffraction peak, △ is thing phase diffraction peak;
Fig. 2 is resistance and the 1000/T graph of a relation of the invention process 1 gained orientation thermosensitive film resistance.
Embodiment
Embodiment 1
A, for La:Mn:Al=1:0.6:0.4, lanthanum nitrate, manganous acetate and aluminum nitrate are dissolved in respectively in Glacial acetic acid and ethylene glycol monomethyl ether in molar ratio, wherein the volume ratio of Glacial acetic acid and ethylene glycol monomethyl ether is 1:1, is then heated to temperature 60 C, stir, to be dissolved complete, stop heating, be cooled to room temperature;
B, three kinds of solution in step a are mixed again, continue to stir 6h, being modulated into concentration is 0.1mol/L solution, filters, and leaves standstill 8h, forms manganese lanthanum aluminate colloidal sol;
C, utilize spin-coating method, under room temperature, step b manganese lanthanum aluminate colloidal sol is dropped in the nickel acid lanthanum substrate of (100) orientation, even glue 20s on sol evenning machine, rotating speed is 3500r/min, then in tube furnace, keep 3min, treatment temp is 300 DEG C, the organism in volatilization film, repeat even glue masking, obtain the film of 150-1500nm thickness;
D, the film that step c is obtained leave standstill and process 1h at 750 DEG C of temperature, are orientated uniformly thermosensitive film, and then sputter gold electrode on ion sputtering instrument leaves standstill 10min at 200 DEG C of temperature, then welds Pt lead-in wire, can obtain thin-film thermistor.
Embodiment 2
A, for La:Mn:Al=1:0.7:0.3, lanthanum nitrate, manganous acetate and aluminum nitrate are dissolved in respectively in Glacial acetic acid and ethylene glycol monomethyl ether in molar ratio, wherein the volume ratio of Glacial acetic acid and ethylene glycol monomethyl ether is 1:1, is then heated to temperature 60 C, stir, to be dissolved complete, stop heating, be cooled to room temperature;
B, three kinds of solution in step a are mixed again, continue to stir 6h, being modulated into concentration is 0.05mol/L solution, filters, and leaves standstill 8h, forms manganese lanthanum aluminate colloidal sol;
C, utilize spin-coating method, under room temperature, step b manganese lanthanum aluminate colloidal sol is dropped in the nickel acid lanthanum substrate of (100) orientation, even glue 20s on sol evenning machine, rotating speed is 3500r/min, then in tube furnace, keep 3min, treatment temp is 300 DEG C, the organism in volatilization film, repeat even glue masking, obtain the film of 150-1500nm thickness;
D, the film that step c is obtained leave standstill and process 1h at 750 DEG C of temperature, are orientated uniformly thermosensitive film, and then sputter gold electrode on ion sputtering instrument leaves standstill 10min at 200 DEG C of temperature, then welds Pt lead-in wire, can obtain thin-film thermistor.
Embodiment 3
A, for La:Mn:Al=1:0.5:0.5, lanthanum nitrate, manganous acetate and aluminum nitrate are dissolved in respectively in Glacial acetic acid and ethylene glycol monomethyl ether in molar ratio, wherein the volume ratio of Glacial acetic acid and ethylene glycol monomethyl ether is 1:1, is then heated to temperature 60 C, stir, to be dissolved complete, stop heating, be cooled to room temperature;
B, three kinds of solution in step a are mixed again, continue to stir 6h, being modulated into concentration is 0.15mol/L solution, filters, and leaves standstill 8h, forms manganese lanthanum aluminate colloidal sol;
C, utilize spin-coating method, under room temperature, step b manganese lanthanum aluminate colloidal sol is dropped in the nickel acid lanthanum substrate of (100) orientation, even glue 20s on sol evenning machine, rotating speed is 3500r/min, then in tube furnace, keep 3min, treatment temp is 300 DEG C, the organism in volatilization film, repeat even glue masking, obtain the film of 150-1500nm thickness;
The film that d obtains step c leaves standstill and processes 1h at 750 DEG C of temperature, is orientated uniformly thermosensitive film, and then sputter gold electrode on ion sputtering instrument leaves standstill 10min at 200 DEG C of temperature, then welds Pt lead-in wire, can obtain thin-film thermistor.
Embodiment 4
A, for La:Mn:Al=1:0.4:0.6, lanthanum nitrate, manganous acetate and aluminum nitrate are dissolved in respectively in Glacial acetic acid and ethylene glycol monomethyl ether in molar ratio, wherein the volume ratio of Glacial acetic acid and ethylene glycol monomethyl ether is 1:1, is then heated to temperature 60 C, stir, to be dissolved complete, stop heating, be cooled to room temperature;
B, three kinds of solution in step a are mixed again, continue to stir 6h, being modulated into concentration is 0.2mol/L solution, filters, and leaves standstill 8h, forms manganese lanthanum aluminate colloidal sol;
C, utilize spin-coating method, under room temperature, step b manganese lanthanum aluminate colloidal sol is dropped in the nickel acid lanthanum substrate of (100) orientation, even glue 20s on sol evenning machine, rotating speed is 3500r/min, then in tube furnace, keep 3min, treatment temp is 300 DEG C, the organism in volatilization film, repeat even glue masking, obtain the film of 150-1500nm thickness;
The film that d obtains step c leaves standstill and processes 1h at 750 DEG C of temperature, can be orientated uniformly thermosensitive film, and then sputter gold electrode on ion sputtering instrument leaves standstill 10min at 200 DEG C of temperature, then welds Pt lead-in wire, can obtain thin-film thermistor.
Embodiment 5
The 1-4 parameter list 1 such as orientation thermosensitive film room temperature resistivity, B value of acquisition arbitrarily will be implemented
As known from Table 1, in embodiment 1, the thin-film thermistor that is La:Mn:Al=1:0.6:0.4 for component, its performance index parameter display, can be for hot environment, therefore, prepares integrated, fast-response high temperature film thermistor with this material component.
Claims (2)
1. be orientated a preparation method for thermosensitive film resistance, it is characterized in that following these steps to carrying out:
A, lanthanum nitrate, manganous acetate and aluminum nitrate are made to raw material, be dissolved in respectively in Glacial acetic acid and ethylene glycol monomethyl ether in, wherein the volume ratio of Glacial acetic acid and ethylene glycol monomethyl ether is 1:1, then at temperature 60-90 DEG C, stir, to be dissolved complete, stop heating, be cooled to room temperature;
B, three kinds of solution in step a are mixed again, continue to stir 6h, being modulated into concentration is 0.05-0.2mol/L solution, filters, and leaves standstill 8h, forms manganese lanthanum aluminate colloidal sol;
C, utilize spin-coating method, under room temperature, step b manganese lanthanum aluminate colloidal sol is dropped in the nickel acid lanthanum substrate of (100) orientation, even glue 20s on sol evenning machine, rotating speed is 3500r/min, then in tube furnace, keep 3min, treatment temp is 300 DEG C, the organism in volatilization film, repeat even glue masking, obtain the film of 150-1500nm thickness;
D, the film that step c is obtained leave standstill and process 1h at 750 DEG C of temperature, are orientated uniformly thermosensitive film, and then sputter gold electrode on ion sputtering instrument leaves standstill 10min at 200 DEG C of temperature, then welds Pt lead-in wire, can obtain thin-film thermistor.
2. method according to claim 1, is characterized in that the mol ratio of step a Raw lanthanum nitrate, manganous acetate and aluminum nitrate is La:Mn:Al=1:0.4-0.7:0.3-0.6.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104266759A (en) * | 2014-10-22 | 2015-01-07 | 中国科学院新疆理化技术研究所 | Function of manganese aluminum acid lanthanum thin film material in intermediate infrared thermosensitive detection |
| CN106835081A (en) * | 2017-02-28 | 2017-06-13 | 宁夏大学 | The preparation method of NTC thermosensitive material films |
| CN113257503A (en) * | 2021-05-13 | 2021-08-13 | 中国科学院新疆理化技术研究所 | All-inorganic flexible thermosensitive device and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102136343A (en) * | 2011-01-21 | 2011-07-27 | 北京鼎臣超导科技有限公司 | Perovskite structure film with giant magneto-impedance effect and preparation method thereof |
| CN103664173A (en) * | 2013-12-17 | 2014-03-26 | 中国科学院新疆理化技术研究所 | Preparation method of high-temperature thick-film thermistor |
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2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102136343A (en) * | 2011-01-21 | 2011-07-27 | 北京鼎臣超导科技有限公司 | Perovskite structure film with giant magneto-impedance effect and preparation method thereof |
| CN103664173A (en) * | 2013-12-17 | 2014-03-26 | 中国科学院新疆理化技术研究所 | Preparation method of high-temperature thick-film thermistor |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104266759A (en) * | 2014-10-22 | 2015-01-07 | 中国科学院新疆理化技术研究所 | Function of manganese aluminum acid lanthanum thin film material in intermediate infrared thermosensitive detection |
| CN106835081A (en) * | 2017-02-28 | 2017-06-13 | 宁夏大学 | The preparation method of NTC thermosensitive material films |
| CN113257503A (en) * | 2021-05-13 | 2021-08-13 | 中国科学院新疆理化技术研究所 | All-inorganic flexible thermosensitive device and preparation method thereof |
| CN113257503B (en) * | 2021-05-13 | 2023-01-03 | 中国科学院新疆理化技术研究所 | All-inorganic flexible thermosensitive device and preparation method thereof |
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