CN112663002A - Thermistor film preparation method based on direct-current reactive co-sputtering - Google Patents
Thermistor film preparation method based on direct-current reactive co-sputtering Download PDFInfo
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- CN112663002A CN112663002A CN202010922184.2A CN202010922184A CN112663002A CN 112663002 A CN112663002 A CN 112663002A CN 202010922184 A CN202010922184 A CN 202010922184A CN 112663002 A CN112663002 A CN 112663002A
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- 238000004544 sputter deposition Methods 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000010408 film Substances 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 29
- 239000000956 alloy Substances 0.000 claims description 25
- 229910045601 alloy Inorganic materials 0.000 claims description 25
- 238000000137 annealing Methods 0.000 claims description 24
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 229910044991 metal oxide Inorganic materials 0.000 claims description 12
- 150000004706 metal oxides Chemical class 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000010409 thin film Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000002739 metals Chemical class 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 description 10
- 239000013077 target material Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 238000001755 magnetron sputter deposition Methods 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 238000005234 chemical deposition Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000010354 integration Effects 0.000 description 3
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Abstract
The invention provides a thermistor film preparation method based on direct-current reactive co-sputtering, which uses Mn1.56Co0.96Ni0.48The preparation method of the thermistor film has the advantages of short time period, low cost, simplicity and convenience.
Description
Technical Field
The invention belongs to the technical field of thermistor film preparation, and particularly relates to a thermistor film preparation method based on direct-current reactive co-sputtering.
Background
With the development of electronic information technology, electronic devices that integrate multiple functions and high integration are widely used in the fields of manufacturing, personal consumption, and the like, so that electronic components are developed toward miniaturization, functionalization, high power, greening, and low cost. Among them, a thermistor is a typical example, and is facing the opportunity of continuously progressing transformation from a traditional discrete component to miniaturization, high reliability, and convenience for integration. In recent years, researchers in the field of thermistors have been focusing on the preparation and performance studies of thermosensitive thin films having the advantages of small size and easy integration. Among them, the MnCoNiO thermal sensitive film material is very suitable to be developed into an integrated temperature sensor with fast response, high sensitivity due to the characteristics of ultra-fast temperature response and stable electrical property, and therefore, the MnCoNiO thermal sensitive film material also receives high attention from domestic and foreign research institutions.
The methods for preparing thermosensitive films adopted by researchers can be divided into two main categories, namely physical deposition methods and chemical deposition methods. The physical deposition method comprises magnetron sputtering, pulsed laser deposition, laser molecular beam epitaxy and the like, and the method has the characteristics that the prepared film material has higher quality and stability, the preparation process is simple and has high repeatability, but the preparation cost is slightly higher; the chemical deposition method comprises chemical solution deposition, screen printing, 3D printing and the like, and the method has the characteristics of low preparation cost, but the process repeatability is not ideal due to the participation of artificial parameters in the process. Therefore, it is a significant task to reduce the cost of physical deposition and to improve the process repeatability of chemical deposition.
The invention aims to reduce the time period and the cost for preparing the thermosensitive film by the traditional magnetron sputtering method. Generally, researchers use traditional rf sputtering methods to prepare thermosensitive thin films, and the first step is to prepare suitable oxide ceramic targets according to the structure and performance characteristics of the prepared thin films. Firstly, the ceramic target material needs to be prepared by adopting a traditional ceramic preparation method; secondly, the size requirement and the density requirement of the target are high, so that the preparation difficulty is higher than that of common ceramics, and the preparation period is longer than that of the common ceramics; and thirdly, preparing a corresponding ceramic target material is needed to prepare each thermosensitive film, and a large amount of manpower and material resources are input particularly in a formula groping stage. In summary, we have found that researchers have to devote a lot of time and effort and materials to the preparation of target materials only when the film preparation has not yet begun to be formally prepared. In addition, the rf magnetron sputtering has a great characteristic of high sputtering quality but low deposition efficiency, and the growth time of the thin film often needs more than several hours, which means that the power energy and the reaction gas need to be consumed more than several hours in each preparation process. This adds virtually to the cost.
In order to avoid the problems, the invention adopts a direct current reaction co-sputtering technology to prepare the metal oxide thermistor film.
Disclosure of Invention
Based on the problems in the prior art, the invention provides a thermistor film preparation method based on direct-current reactive co-sputtering, and Mn is used in the method1.56Co0.96Ni0.48The preparation method of the thermistor film has the advantages of short time period, low cost, simplicity and convenience.
A thermistor film preparation method based on direct current reactive co-sputtering comprises the following steps:
step S10, selecting Mn1.56Co0.96Ni0.48The alloy is used as a basic alloy target, and one or two metals of Mg, Al, Fe, Co and Zn are used as a doped metal target;
step S20, respectively placing the basic alloy target and the doped metal target on different cathode target positions in the sputtering cavity, and placing the cleaned substrate on a sample table;
step S30, replacing the ambient gas in the sputtering cavity with argon as sputtering pressure, heating the substrate and triggering sputtering, controlling the sputtering power of the basic alloy target to be 30-50W, controlling the sputtering power of the doped metal target to be 1-20W, and controlling the sputtering time to be 5-30 min;
and step S40, putting the sample obtained by sputtering deposition in the step S30 into an oxygen atmosphere annealing furnace for annealing to obtain the metal oxide heat-sensitive film.
Wherein the step S30 includes a step S31 of pumping out air in the sputtering chamber until the air pressure is lower than 10 < -3 > Pa, and then refilling argon gas with purity higher than 99.9%.
Wherein, the purity of the base alloy target and the doped metal target in the step S10 is over 99%, the diameter is 100mm, and the thickness is 1 mm.
Wherein the heating temperature of the substrate in the step S30 is 100-300 ℃, and the sputtering pressure in the sputtering cavity is 1-10 Pa.
Wherein, the annealing conditions in step S40 are: the annealing temperature is 500-900 ℃, the oxygen pressure is 1-105 Pa, and the annealing time is 20-60 min.
Wherein the substrate in step S20 is a silicon wafer (SiO) with a silicon dioxide layer2/Si) or silicon wafers with silicon nitride layers (Si)3N4/Si) or AlN polycrystalline ceramic wafer.
The invention has the beneficial effects that:
1. the method disclosed by the invention comprises the following steps of firstly, selecting a proper basic alloy target and a proper doped metal target; then, the selected target materials are placed on a plurality of sputtering target positions at the same time, and the film deposition substrate is placed on a sample table; then adjusting sputtering parameters including substrate temperature, sputtering air pressure, sputtering power and sputtering time, thereby realizing glow starting sputtering of a plurality of targets; finally, the substrate deposited with the film material is placed in oxygen for annealing treatment, and the metal oxide thermosensitive film is obtained, compared with the traditional magnetron sputtering method, the method has the difference that more anode working target materials are provided, and then a more complex sputtering process is formed, different target material particles move and interact simultaneously in the sputtering process, and the interaction when various particles fall on the film deposition substrate makes the distribution of all materials of the film more uniform and has better combination effect; the basic alloy target is an alloy mixture target with heat-sensitive characteristics, the proportion of each element in the film can be adjusted by adjusting the type and power of the doped metal target, and a serialized film material with adjustable electrical parameters in a large range is prepared, so that the method is very suitable for designing and developing a new heat-sensitive film material.
2. The method for preparing the metal oxide thermistor film has the characteristics of short time period, low cost, simplicity, convenience and the like, solves the problem that the thermistor film is difficult to coexist with high quality and low cost in the process of changing from basic research to practical research, and has universality for development of various film type thermistors.
Drawings
FIG. 1 is an XRD pattern of a thermosensitive thin film prepared by a method for preparing a metal oxide thermosensitive resistance thin film based on a direct current reactive co-sputtering technique;
FIG. 2 is an SEM image of a thermosensitive film prepared by the method for preparing a metal oxide thermosensitive resistor film based on a direct-current reactive co-sputtering technique;
FIG. 3 is a temperature resistance relationship diagram of a thermosensitive film prepared by the method for preparing a metal oxide thermosensitive resistance film based on the direct-current reactive co-sputtering technique.
Detailed Description
The invention is described in detail below with reference to the figures and the specific embodiments.
The first embodiment is as follows:
a thermistor film preparation method based on direct current reactive co-sputtering comprises the following steps:
step S10, selecting Mn1.56Co0.96Ni0.48The alloy is used as a basic alloy target, two metals of Mg and Al are used as a doping metal target, the purity of the target material exceeds 99 percent, the diameter is 100mm, and the thickness is 1 mm;
step S20, respectively placing the selected MnCoNi alloy target, the Mg target and the Al target on three different cathode target positions in a sputtering cavity, and cleaning the targetsSiO of (2)2the/Si substrate is placed on a sample table;
step S30, pumping out air in the sputtering chamber until the air pressure is lower than 10-3Pa, refilling argon with the purity of more than 99.9 percent until the air pressure is 1Pa, heating the substrate to 100 ℃ and triggering sputtering, controlling the sputtering power of the basic alloy target to be 30W, controlling the sputtering power of the Mg target to be 1W, controlling the sputtering power of the Al target to be 20W, and controlling the sputtering time to be 5 min;
and step S40, putting the sample obtained by sputtering deposition in the step S30 into an oxygen atmosphere annealing furnace for annealing, and annealing for 20min under the conditions of the annealing temperature of 500 ℃ and the oxygen pressure of 1Pa to obtain the MnCoNiMgAlO metal oxide heat-sensitive film.
Example two:
a thermistor film preparation method based on direct current reactive co-sputtering comprises the following steps:
step S10, selecting MnCoNi alloy as a basic alloy target, and then using Zn metal as a doped metal target, wherein the purity of the target exceeds 99%, the diameter is 100mm, and the thickness is 1 mm;
step S20, respectively placing the selected MnCoNi alloy target and the Zn target on two different cathode targets in a sputtering cavity, and cleaning the Si3N4the/Si substrate is placed on a sample table;
step S30, pumping out air in the sputtering chamber until the air pressure is lower than 10-3Pa, refilling argon with the purity of more than 99.9 percent until the air pressure is 10Pa, heating the substrate to 300 ℃ and triggering sputtering, controlling the sputtering power of the basic alloy target to be 50W, controlling the sputtering power of the Zn target to be 10W, and controlling the sputtering time to be 30 min;
step S40, putting the sample obtained by sputtering deposition in the step S30 into an oxygen atmosphere annealing furnace for annealing, wherein the annealing temperature is 900 ℃ and the oxygen pressure is 10 DEG C5Annealing for 60min under the condition of Pa to obtain the MnCoNiZnO metal oxide heat-sensitive film.
Example three:
a thermistor film preparation method based on direct current reactive co-sputtering comprises the following steps:
step S10, selecting MnCoNi alloy as a basic alloy target, and then using two metals of Cu and Fe as a doped metal target, wherein the purity of the target exceeds 99%, the diameter is 100mm, and the thickness is 1 mm;
s20, respectively placing the selected MnCoNi alloy target, the Cu target and the Fe target on three different cathode target positions in a sputtering cavity, and placing the cleaned AlN ceramic substrate on a sample table;
step S30, pumping out air in the sputtering chamber until the air pressure is lower than 10-3Pa, refilling argon with the purity of more than 99.9 percent until the air pressure is 5Pa, heating the substrate to 200 ℃ and triggering sputtering, controlling the sputtering power of the basic alloy target to be 40W, controlling the sputtering power of the Cu target to be 15W, controlling the sputtering power of the Fe target to be 5W, and controlling the sputtering time to be 20 min;
and step S40, putting the sample obtained by sputtering deposition in the step S30 into an oxygen atmosphere annealing furnace for annealing, and annealing for 30min under the annealing conditions of the annealing temperature of 750 ℃ and the oxygen pressure of 100Pa to obtain the MnCoNiCuFeO metal oxide heat-sensitive film.
XRD, SEM and electrical property tests of the thermosensitive thin film material obtained in any one of the first, second and third examples are shown in FIGS. 1 to 3. As can be seen from the figure, the thermosensitive film prepared by the method for preparing the metal oxide thermosensitive resistance film based on the direct-current reactive co-sputtering technology has the characteristics of good crystallinity, high density, controllable electrical property parameters and the like.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. A thermistor film preparation method based on direct current reactive co-sputtering is characterized by comprising the following steps:
step S10, selecting Mn1.56Co0.96Ni0.48The alloy is used as a basic alloy target, and one or two metals of Mg, Al, Fe, Co and Zn are used as a doped metal target;
step S20, respectively placing the basic alloy target and the doped metal target on different cathode target positions in the sputtering cavity, and placing the cleaned substrate on a sample table;
step S30, replacing the ambient gas in the sputtering cavity with argon as sputtering pressure, heating the substrate and triggering sputtering, controlling the sputtering power of the basic alloy target to be 30-50W, controlling the sputtering power of the doped metal target to be 1-20W, and controlling the sputtering time to be 5-30 min;
and step S40, putting the sample obtained by sputtering deposition in the step S30 into an oxygen atmosphere annealing furnace for annealing to obtain the metal oxide heat-sensitive film.
2. The method of claim 1, wherein the step S30 includes a step S31, the air in the sputtering chamber is pumped to a pressure lower than 10%-3Pa, and then argon with the purity of more than 99.9 percent is filled again.
3. The method of claim 2, wherein the purity of the base alloy target and the doped metal target in step S10 is more than 99%, the diameter is 100mm, and the thickness is 1 mm.
4. The method for preparing a thermistor thin film based on DC reactive co-sputtering as claimed in claim 2, wherein the heating temperature of the substrate in step S30 is 100 ℃ to 300 ℃, and the sputtering pressure in the sputtering chamber is 1Pa to 10 Pa.
5. The method for preparing a thermistor thin film based on dc reactive co-sputtering according to any of claims 1-4, wherein the annealing conditions in step S40 are: the annealing temperature is 500-900 ℃, the oxygen pressure is 1-105 Pa, and the annealing time is 20-60 min.
6. The method for preparing a thermistor thin film based on DC reactive co-sputtering according to any of claims 1-4, wherein the substrate in step S20 is a silicon wafer with a silicon dioxide layer or a silicon wafer with a silicon nitride layer or an AlN polycrystalline ceramic wafer.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107881475A (en) * | 2016-09-30 | 2018-04-06 | 江西理工大学 | A kind of method that Ni Co Mn Ti alloy firms are prepared by magnetron sputtering DC sputturing method |
| CN109735807A (en) * | 2019-02-27 | 2019-05-10 | 华中科技大学 | A kind of preparation method of negative temperature coefficient heat-sensitive film |
| CN110106485A (en) * | 2019-05-18 | 2019-08-09 | 中国科学院新疆理化技术研究所 | A kind of negative temperature coefficient heat-sensitive film and preparation method thereof |
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2020
- 2020-09-04 CN CN202010922184.2A patent/CN112663002A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107881475A (en) * | 2016-09-30 | 2018-04-06 | 江西理工大学 | A kind of method that Ni Co Mn Ti alloy firms are prepared by magnetron sputtering DC sputturing method |
| CN109735807A (en) * | 2019-02-27 | 2019-05-10 | 华中科技大学 | A kind of preparation method of negative temperature coefficient heat-sensitive film |
| CN110106485A (en) * | 2019-05-18 | 2019-08-09 | 中国科学院新疆理化技术研究所 | A kind of negative temperature coefficient heat-sensitive film and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| TINGTING XUAN等: ""Characterization of Al-doped Mn-Co-Ni-O NTC thermistor films prepared by the magnetron co-sputtering approach"", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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Application publication date: 20210416 |