CN206990123U - A kind of low temperature temperature element based on layered cobalt oxide - Google Patents
A kind of low temperature temperature element based on layered cobalt oxide Download PDFInfo
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- CN206990123U CN206990123U CN201720651656.9U CN201720651656U CN206990123U CN 206990123 U CN206990123 U CN 206990123U CN 201720651656 U CN201720651656 U CN 201720651656U CN 206990123 U CN206990123 U CN 206990123U
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- 229910000428 cobalt oxide Inorganic materials 0.000 title claims abstract description 27
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 151
- 239000002184 metal Substances 0.000 claims abstract description 151
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims description 14
- 229910002244 LaAlO3 Inorganic materials 0.000 claims description 4
- 229910018307 LaxSr1−x Inorganic materials 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 229910002367 SrTiO Inorganic materials 0.000 claims 1
- -1 cobalt oxide Compound Chemical class 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 43
- 238000000137 annealing Methods 0.000 description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 12
- 239000000843 powder Substances 0.000 description 8
- 239000010409 thin film Substances 0.000 description 8
- 238000011065 in-situ storage Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 238000004549 pulsed laser deposition Methods 0.000 description 5
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229910002370 SrTiO3 Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006903 response to temperature Effects 0.000 description 2
- 229910002372 SrTiO3(001) Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
Abstract
The utility model discloses a kind of low temperature temperature element based on layered cobalt oxide, including single crystal substrates, film temperature-sensitive element, metal electrode I, metal electrode II, metal electrode III, metal electrode IV, wire I, wire II, film temperature-sensitive element is on single-crystal substrates along c-axis epitaxial growth, the metal electrode I of equidistant arrangement is disposed with film temperature-sensitive element upper surface, metal electrode II, metal electrode III, metal electrode IV, metal electrode I, metal electrode IV connects constant current source output terminal by wire I, metal electrode II, metal electrode III connects voltmeter input by wire II, film temperature-sensitive element is layered cobalt oxide film；The utility model temperature element temperature-coefficient of electrical resistance at 0 DEG C ~ 200 DEG C is big, resistance temperature relation good linearity, and physical and chemical performance is stable, cost is cheap.
Description
Technical field
A kind of low temperature temperature element based on layered cobalt oxide is the utility model is related to, belongs to detecting devices technology neck
Domain.
Background technology
Currently for -100 DEG C and following low temperature accurate measurement, industrial most widely used temperature element is Pt100,
That is the platinum resistance thermometer sensor, of purity >=99.9995%, this has higher temperature-coefficient of electrical resistance (TCR) ~ 0.374% (0 mainly due to Pt
DEG C), make its detectivity high, and it is approximately linear relationship in low temperature range internal resistance value and temperature, is easy to index and reads
Number.But it still has numerous deficiencies, such as：Pt is easily reduced pollution in reducing atmosphere, become fragile, it is necessary to is isolated with protection sleeve pipe
Harmful atmosphere；Resistivity is smaller, and ρ (0 DEG C) is only 9.8 × 10-3M Ω cm, make the thermoelectricity resistance body in the case where exporting identical voltage signal
Product is big, causes its thermal capacity and thermal inertia big, the response to temperature fluctuation is slower；Earth reserves are small, and price is high.
The content of the invention
In view of the above-mentioned problems, the utility model provides a kind of low temperature temperature element based on layered cobalt oxide, including list
Brilliant substrate, film temperature-sensitive element, metal electrode I, metal electrode II, metal electrode III, metal electrode IV, wire I, wire II,
Along c-axis epitaxial growth, equidistant arrangement is disposed with film temperature-sensitive element upper surface on single-crystal substrates for film temperature-sensitive element
Metal electrode I, metal electrode II, metal electrode III, metal electrode IV, metal electrode I, metal electrode IV are connected by wire I
Constant current source output terminal is connect, metal electrode II, metal electrode III connect voltmeter input by wire II, and film temperature-sensitive element is
Layered cobalt oxide film.
The single crystal substrates are (00l) orientation SrTiO3、LaAlO3Or (LaxSr1-x)(AlyTa1-y)O3, (LaxSr1-x)
(AlyTa1-y)O3In 0.1≤x≤0.5,0.5≤y≤0.7.
The metal electrode I, metal electrode II, metal electrode III, the material of metal electrode IV are identical, be Ag, Cu, In or
Pt, the spacing 1-5mm between metal electrode I, metal electrode II, metal electrode III, metal electrode IV.
The wire I, the material therefor of wire II are identical, are Ag or Cu wires, wire 1, a diameter of 0.05- of wire 2
0.2mm。
Layered cobalt oxide films are stratiform Ca3Co4O9+δFilm, Ca3Co4O9+δFilm can be according to prior art
It is prepared, can also be prepared using the following steps：
A, the preparation of layered cobalt oxide polycrystalline bulk：By the CaCO that purity is 99.99%3、Co3O4Massage that ratio
Ca:Co=3:4 mixing, grinding 5-10h, after 10-20MPa uniaxial tensions push sheetmolding at air atmosphere, 800-850 DEG C
Pre-burning 12-24h, 5-10h is then re-grind into powder, sheetmolding is pushed in 10-20MPa uniaxial tensions, in air atmosphere, 880-
24-36h is sintered at 900 DEG C, obtains Ca3Co4O9+δPolycrystalline bulk, the amount of oxygen atom is left 9 in 9+ δ ability domain representation chemical formulas
It is right；
B, the preparation of epitaxial film：The polycrystalline bulk obtained using step A is target, with pulsed laser deposition in single crystal substrates
Upper growth performed thin film；
C, in-situ annealing：By the performed thin film that step B is obtained under static oxygen atmosphere in-situ annealing, obtain c-axis extension
Layered cobalt oxide film.
The process conditions of pulsed laser deposition described in step B are KrF PRK wavelength 248nm, laser pulse width
28ns, laser energy density 1-2.5 mJ/cm2, laser frequency 2-5Hz, back end vacuum 10-4-10-5Pa, growth temperature 760-800
DEG C, growth flowing oxygen pressure 20-40Pa, growth time 10-40min.
The technique of in-situ annealing described in step C is 780-820 DEG C of annealing temperature, annealing oxygen pressure 2 × 104- 4×104Pa,
Annealing time 10-30min.
The beneficial effects of the utility model are：
Physical and chemical performance is stable in temperature-measuring range；Temperature-coefficient of electrical resistance TCR is sensitive up to 0.49% (0 DEG C), detection
Degree is high；Resistivity-temperature linearity is on speaking terms in 30 DEG C ~ -180 DEG C whole temperature ranges, is easy to indexing, reading；There is larger electricity
Resistance rate ρ (0 DEG C) ≈ 4.5-5m Ω cm, 3 orders of magnitude bigger than Pt100, therefore under identical output voltage, the volume and use of element
Material is significantly small, and thermal capacity and thermal inertia are small, and the response to temperature change is faster；Layered cobalt oxide material anisotropy, and make
Standby raw material is common oxide powder, and cost is cheap.
Brief description of the drawings
Fig. 1 is the cross-sectional view of the utility model low temperature temperature element；
Fig. 2 is resistivity-temperature curve of low temperature temperature element in the utility model embodiment 1；
Fig. 3 is resistivity-temperature curve of low temperature temperature element in the utility model embodiment 2；
In Fig. 1：1- single crystal substrates, 2- film temperature-sensitive elements, 3- wires I, 4- wires II, 5- metal electrodes I, 6- metals electricity
Pole II, 7- metal electrodes III, 8- metal electrodes IV.
Embodiment
The utility model is further described with specific embodiment below in conjunction with the accompanying drawings, but protection of the present utility model
Scope is not limited to the content.
Embodiment 1
A kind of low temperature temperature element based on layered cobalt oxide, as shown in figure 1, including single crystal substrates 1, film thermal element
Part 2, wire I 3, wire II 4, metal electrode I 5, metal electrode II 6, metal electrode III 7, metal electrode IV 8, film thermal element
For part 2 along c-axis epitaxial growth in single crystal substrates 1, equidistant arrangement successively is provided with the upper surface of film temperature-sensitive element 2 has metal electric
Pole I 5, metal electrode II 6, metal electrode III 7, metal electrode IV 8, metal electrode I 5, metal electrode IV 8 are connected by wire I 3
Constant current source output terminal, metal electrode II 6, metal electrode III 7 connect voltmeter input by wire II 4；Film temperature-sensitive element 2
For layered cobalt oxide film.
Single crystal substrates 1 are (00 in the present embodimentl) orientation SrTiO3, metal electrode I 5, metal electrode II 6, metal electricity
Pole III 7, the material of metal electrode IV 8 are identical, are Ag, metal electrode I 5, metal electrode II 6, metal electrode III 7, metal electrode
Spacing 1mm between IV 8；Wire I 3, the material therefor of wire II 4 are identical, are Cu wires, a diameter of 0.05mm.
The layered cobalt oxide films of the present embodiment are stratiform Ca3Co4O9+δFilm, its preparation method specifically include following
Step：
A、Ca3Co4O9+δThe preparation of polycrystalline bulk：Using solid reaction process, by the CaCO that purity is 99.99%3、Co3O4Powder
Last Ca in molar ratio:Co=3:4 mixing, grinding 5h, after 10MPa uniaxial tensions push sheetmolding at air atmosphere, 800 DEG C
Pre-burning 12h, 5h is then re-grind into powder, sheetmolding is pushed in 10MPa uniaxial tensions, is sintered at air atmosphere, 880 DEG C
24h, obtain Ca3Co4O9+δPolycrystalline bulk；
B, the preparation of epitaxial film：The Ca obtained with step A3Co4O9+δPolycrystalline bulk is target, with pulsed laser deposition,
Using process conditions as KrF PRKs wavelength 248nm, laser pulse width 28ns, the mJ/cm of laser energy density 12, laser frequency
2Hz, back end vacuum 10-4Pa, 760 DEG C of growth temperature, growth flowing oxygen pressure 20Pa, growth time 10min, in SrTiO3(001)
Ca is grown in single crystal substrates3Co4O9+δPerformed thin film；
C, in-situ annealing：The Ca that step B is obtained3Co4O9+δPerformed thin film is annealed under static oxygen atmosphere, annealing temperature
780 DEG C, annealing oxygen pressure 2 × 104Pa, annealing time 10min, obtain the stratiform Ca of c-axis extension3Co4O9+δFilm.
The present embodiment element is placed in target thermometric environment, by being inputted between metal electrode I 5, metal electrode IV 8
Known constant-current source, and the voltmeter reading metal electrode II 6, metal electrode III 7, can calculate to obtain member by Ohm's law
Part resistance at such a temperature and resistivity, further compare its resistivity-temperature curve and can obtain test environment temperature.
Resistivity-temperature curve of the present embodiment temperature element in 26 DEG C ~ -173 DEG C temperature ranges is shown in Fig. 2, resistivity -
Temperature relation is almost linear, and temperature-coefficient of electrical resistance TCR is up to 0.49% at 0 DEG C, electricalresistivityρ ≈ 5m Ω cm.
Embodiment 2
A kind of low temperature temperature element based on layered cobalt oxide, including single crystal substrates 1, film temperature-sensitive element 2, wire I
3rd, wire II 4, metal electrode I 5, metal electrode II 6, metal electrode III 7, metal electrode IV 8, film temperature-sensitive element 2 is in monocrystalline
Along c-axis epitaxial growth in substrate 1, the upper surface of film temperature-sensitive element 2, which is provided with equidistant arrangement successively, metal electrode I 5, metal
Electrode II 6, metal electrode III 7, metal electrode IV 8, metal electrode I 5, metal electrode IV 8 are defeated by the connection constant-current source of wire I 3
Go out end, metal electrode II 6, metal electrode III 7 connect voltmeter input by wire II 4；Film temperature-sensitive element 2 is stratiform cobalt
Sull.
Single crystal substrates 1 are (00 in the present embodimentl) orientation LaAlO3, metal electrode I 5, metal electrode II 6, metal electricity
Pole III 7, the material of metal electrode IV 8 are identical, are In, metal electrode I 5, metal electrode II 6, metal electrode III 7, metal electrode
Spacing 3mm between IV 8；Wire I 3, the material therefor of wire II 4 are identical, are Ag wires, a diameter of 0.1mm.
The layered cobalt oxide films of the present embodiment are stratiform Ca3Co4O9+δFilm, its preparation method specifically include following
Step：
A、Ca3Co4O9+δThe preparation of polycrystalline bulk：Using solid reaction process, by the CaCO that purity is 99.99%3、Co3O4Powder
Last Ca in molar ratio:Co=3:4 mixing, grinding 8h, after 15MPa uniaxial tensions push sheetmolding at air atmosphere, 820 DEG C
Pre-burning 20h, 8h is then re-grind into powder, sheetmolding is pushed in 15MPa uniaxial tensions, is sintered at air atmosphere, 890 DEG C
30h, obtain Ca3Co4O9+δPolycrystalline bulk；
B, the preparation of epitaxial film：The Ca obtained with step A3Co4O9+δPolycrystalline bulk is target, with pulsed laser deposition,
Process conditions are KrF PRKs wavelength 248nm, laser pulse width 28ns, the mJ/cm of laser energy density 1.82, laser frequency
3Hz, back end vacuum 10-4Pa, 780 DEG C of growth temperature, growth flowing oxygen pressure 30Pa, growth time 20min, in LaAlO3(001)
Ca is grown in single crystal substrates3Co4O9+δPerformed thin film；
C, in-situ annealing：The Ca that step B is obtained3Co4O9+δPerformed thin film is annealed under static oxygen atmosphere, annealing temperature
800 DEG C, annealing oxygen pressure 3 × 104Pa, annealing time 20min, obtain the stratiform Ca of c-axis extension3Co4O9+δFilm.
The present embodiment element is placed in target thermometric environment, by being inputted between metal electrode I 5, metal electrode IV 8
Known constant-current source, and the voltmeter reading metal electrode II 6, metal electrode III 7, can calculate to obtain member by Ohm's law
Part resistance at such a temperature and resistivity, further compare its resistivity-temperature curve and can obtain test environment temperature.
Resistivity-temperature curve of the present embodiment temperature element in 26 DEG C ~ -173 DEG C temperature ranges is shown in Fig. 2, resistivity -
Temperature relation is almost linear, and 0 DEG C of temperature-coefficient of electrical resistance TCR reaches ~ 0.3%, electricalresistivityρ ≈ 4.5m Ω cm.
Embodiment 3
A kind of low temperature temperature element based on layered cobalt oxide, including single crystal substrates 1, film temperature-sensitive element 2, wire I
3rd, wire II 4, metal electrode I 5, metal electrode II 6, metal electrode III 7, metal electrode IV 8, film temperature-sensitive element 2 is in monocrystalline
Along c-axis epitaxial growth in substrate 1, the upper surface of film temperature-sensitive element 2, which is provided with equidistant arrangement successively, metal electrode I 5, metal
Electrode II 6, metal electrode III 7, metal electrode IV 8, metal electrode I 5, metal electrode IV 8 are defeated by the connection constant-current source of wire I 3
Go out end, metal electrode II 6, metal electrode III 7 connect voltmeter input by wire II 4；Film temperature-sensitive element 2 is stratiform cobalt
Sull.
Single crystal substrates are (00 in the present embodimentl) orientation (La0.3Sr0.7)(Al0.65Ta0.35)O3, metal electrode I 5, gold
It is identical to belong to electrode II 6, metal electrode III 7, the material of metal electrode IV 8, is Pt, metal electrode I 5, metal electrode II 6, metal
Spacing 5mm between electrode III 7, metal electrode IV 8；Wire I 3, the material therefor of wire II 4 are identical, are Ag wires, a diameter of
0.2mm。
The layered cobalt oxide films of the present embodiment are stratiform Ca3Co4O9+δFilm, its preparation method specifically include following
Step：
A、Ca3Co4O9+δThe preparation of polycrystalline bulk：Using solid reaction process, by the CaCO that purity is 99.99%3、Co3O4Powder
Last Ca in molar ratio:Co=3:4 mixing, grinding 10h, after 20MPa uniaxial tensions push sheetmolding at air atmosphere, 850 DEG C
Pre-burning 24h, 10h is then re-grind into powder, sheetmolding is pushed in 20MPa uniaxial tensions, is sintered at air atmosphere, 900 DEG C
36h, obtain Ca3Co4O9+δPolycrystalline bulk；
B, the preparation of epitaxial film：The Ca obtained with step A3Co4O9+δPolycrystalline bulk is target, with pulsed laser deposition,
Process conditions are KrF PRKs wavelength 248nm, laser pulse width 28ns, the mJ/cm of laser energy density 2.52, laser frequency
4Hz, back end vacuum 10-5Pa, 800 DEG C of growth temperature, growth flowing oxygen pressure 40Pa, growth time 40min, in (La0.3Sr0.7)
(Al0.65Ta0.35)O3(001) Ca is grown in single crystal substrates3Co4O9+δPerformed thin film；
C, in-situ annealing：The Ca that step B is obtained3Co4O9+δPerformed thin film is annealed under static oxygen atmosphere, annealing temperature
820 DEG C, annealing oxygen pressure 4 × 104Pa, annealing time 30min, obtain the stratiform Ca of c-axis extension3Co4O9+δFilm.
The present embodiment element is placed in target thermometric environment, by being inputted between metal electrode I 5, metal electrode IV 8
Known constant-current source, and the voltmeter reading metal electrode II 6, metal electrode III 7, can calculate to obtain member by Ohm's law
Part resistance at such a temperature and resistivity, further compare its resistivity-temperature curve and can obtain test environment temperature.
Embodiment 4
A kind of low temperature temperature element based on layered cobalt oxide, including single crystal substrates 1, film temperature-sensitive element 2, wire I
3rd, wire II 4, metal electrode I 5, metal electrode II 6, metal electrode III 7, metal electrode IV 8, film temperature-sensitive element 2 is in monocrystalline
Along c-axis epitaxial growth in substrate 1, the upper surface of film temperature-sensitive element 2, which is provided with equidistant arrangement successively, metal electrode I 5, metal
Electrode II 6, metal electrode III 7, metal electrode IV 8, metal electrode I 5, metal electrode IV 8 are defeated by the connection constant-current source of wire I 3
Go out end, metal electrode II 6, metal electrode III 7 connect voltmeter input by wire II 4；Film temperature-sensitive element 2 is stratiform cobalt
Sull.
Single crystal substrates are (00 in the present embodimentl) orientation (La0.4Sr0.6)(Al0.6Ta0.4)O3, metal electrode I 5, metal
Electrode II 6, metal electrode III 7, the material of metal electrode IV 8 are identical, are In, and metal electrode I 5, metal electrode II 6, metal are electric
Spacing 3mm between pole III 7, metal electrode IV 8；Wire I 3, the material therefor of wire II 4 are identical, are Ag wires, a diameter of
0.15mm。
The layered cobalt oxide films of the present embodiment are stratiform Ca3Co4O9+δFilm, the method with reference to disclosed in prior art
It is prepared（The Ca of c-axis preferentially3Co4O9Polycrystalline, the preparation of film and laser induced thermoelectric voltage experimental study, Kunming science and engineering are big
Master thesis, 2013）.
The present embodiment element is placed in target thermometric environment, by being inputted between metal electrode I 5, metal electrode IV 8
Known constant-current source, and the voltmeter reading metal electrode II 6, metal electrode III 7, can calculate to obtain member by Ohm's law
Part resistance at such a temperature and resistivity, further compare its resistivity-temperature curve and can obtain test environment temperature.
Claims (5)
1. a kind of low temperature temperature element based on layered cobalt oxide, it is characterised in that including single crystal substrates, film thermal element
Part, metal electrode I, metal electrode II, metal electrode III, metal electrode IV, wire I, wire II, film temperature-sensitive element is in monocrystalline
Along c-axis epitaxial growth in substrate, metal electrode I, the metal that equidistant arrangement is disposed with film temperature-sensitive element upper surface are electric
Pole II, metal electrode III, metal electrode IV, metal electrode I, metal electrode IV connect constant current source output terminal, metal by wire I
Electrode II, metal electrode III connect voltmeter input by wire II, and film temperature-sensitive element is layered cobalt oxide film.
2. the low temperature temperature element based on layered cobalt oxide according to claim 1, it is characterised in that the single crystal substrates
For 00lThe SrTiO of orientation3、LaAlO3Or (LaxSr1-x)(AlyTa1-y)O3, (LaxSr1-x)(AlyTa1-y)O3In 0.1≤x≤
0.5,0.5≤y≤0.7.
3. the low temperature temperature element based on layered cobalt oxide according to claim 1, it is characterised in that the metal electrode
Ith, metal electrode II, metal electrode III, the material of metal electrode IV are identical, are Ag, Cu, In or Pt, and metal electrode I, metal are electric
Spacing between pole II, metal electrode III, metal electrode IV is 1-5mm.
4. the low temperature temperature element based on layered cobalt oxide according to claim 1, it is characterised in that the wire I, lead
The material therefor of line II is identical, is Ag or Cu wires, wire I, a diameter of 0.05-0.2mm of wire II.
5. the low temperature temperature element based on layered cobalt oxide according to claim 1, it is characterised in that layered cobalt oxide
Compound film is stratiform Ca3Co4O9+δFilm.
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