CN116283274B - NTC thermistor material based on rare earth element and preparation method thereof - Google Patents
NTC thermistor material based on rare earth element and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 54
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 35
- 238000000498 ball milling Methods 0.000 claims abstract description 27
- 239000000084 colloidal system Substances 0.000 claims abstract description 21
- 238000004108 freeze drying Methods 0.000 claims abstract description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 18
- 239000011230 binding agent Substances 0.000 claims abstract description 17
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 11
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 17
- 238000000227 grinding Methods 0.000 claims description 17
- 229910052760 oxygen Inorganic materials 0.000 claims description 17
- 239000001301 oxygen Substances 0.000 claims description 17
- 229910002651 NO3 Inorganic materials 0.000 claims description 15
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 15
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 14
- GNMQOUGYKPVJRR-UHFFFAOYSA-N nickel(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ni+3].[Ni+3] GNMQOUGYKPVJRR-UHFFFAOYSA-N 0.000 claims description 14
- 238000003825 pressing Methods 0.000 claims description 13
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 239000011268 mixed slurry Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000395 magnesium oxide Substances 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 7
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 5
- 238000009694 cold isostatic pressing Methods 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 5
- 235000015110 jellies Nutrition 0.000 claims description 5
- 239000008274 jelly Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052773 Promethium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 2
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 claims description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- 239000000499 gel Substances 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 206010057040 Temperature intolerance Diseases 0.000 description 3
- 210000001072 colon Anatomy 0.000 description 3
- 230000008543 heat sensitivity Effects 0.000 description 3
- 238000009529 body temperature measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008542 thermal sensitivity Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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Abstract
The invention provides an NTC thermistor material based on rare earth elements and a preparation method thereof. The preparation method of the NTC thermistor material based on the rare earth element comprises the following steps: dissolving metal oxide with nitric acid, freeze drying colloid, doping BaTiO 3 Ball milling, adding binder and sintering. The invention has stable high-temperature structure and better thermosensitive property by doping BaTiO 3 The ball milling is carried out, so that the prepared NTC thermistor has stable phase structure at high temperature, has the function of measuring temperature in a high-temperature wide temperature area, and effectively widens the applicability of the NTC thermistor, thereby ensuring the measurement accuracy of the NTC thermistor.
Description
Technical Field
The invention relates to the technical field of NTC (negative temperature coefficient) thermosensitive materials, in particular to an NTC thermosensitive resistor material based on rare earth elements and a preparation method thereof.
Background
NTC thermistor has many advantages such as sensitive to temperature, small, respond fast and interchangeability, is widely used in aspects such as temperature measurement, temperature control and temperature compensation, but because NTC thermistor material phase structure is unstable under high temperature, and the thermal sensitivity is relatively poor, leads to its use warm area to be limited, is difficult to be applied in fields such as electron, military and aerospace that need high temperature measurement for NTC thermistor's suitability is not extensive enough.
The foregoing is provided merely for the purpose of facilitating understanding of the technical solutions of the present invention and is not intended to represent an admission that the foregoing is prior art.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide an NTC thermistor material based on rare earth elements and a preparation method thereof.
A preparation method of an NTC thermistor material based on rare earth elements comprises the following steps:
s1: dissolution of metal oxides with nitric acid
Adding magnesium oxide, manganese dioxide, nickel sesquioxide, ferric oxide and rare earth oxide into a nitric acid solution, stirring and dissolving, adding an ethanol solution, stirring and mixing, adding triethanolamine to adjust pH, stirring, and standing to obtain a colloid;
s2: freeze-dried jelly
Freeze-drying the colloid, grinding, uniformly dispersing, calcining, and cooling to room temperature to obtain an intermediate A;
s3: doped BaTiO 3 Ball milling
Adding absolute ethyl alcohol into the intermediate A, ball milling, and then adding BaTiO 3 Continuing ball milling, and then drying, grinding and sieving to obtain an intermediate B;
s4: adding binder and sintering
And adding a binder into the intermediate B, uniformly mixing, pressing into a wafer, sintering at a high temperature, and naturally cooling to obtain the NTC thermistor material based on the rare earth elements.
Further, the step S1 of dissolving the metal oxide with nitric acid specifically includes the following steps:
s1.1: adding magnesium oxide, manganese dioxide, nickel sesquioxide, ferric oxide and rare earth oxide into a reaction box containing nitric acid solution according to the mass ratio of 5-7:15-22:17-25:5-10:2-3, and stirring and dissolving by using a stirrer to obtain nitrate solution;
s1.2: filling absolute ethyl alcohol into a stirrer, and introducing the absolute ethyl alcohol into the nitrate solution from a one-way through hole on a stirring rod while stirring by the stirrer;
s1.3: after the absolute ethyl alcohol and the nitrate solution are uniformly mixed, the triethanolamine is pressed into the reaction box from the small holes on the inner wall of the reaction box through a hydraulic pump, and is stirred for 3 to 5 hours at the speed of 300 to 500 r/min;
s1.4: and (3) detecting the pH value in the reaction tank in real time by a pH detector in the reaction tank until the pH value in the reaction tank is=6-7, stopping adding triethanolamine, stopping stirring, and standing for 2-3 hours to obtain a colloid.
Further, the freeze-drying colloid in the step S2 specifically includes the following steps:
s2.1: placing the colloid in a freeze drying box, cooling to-25 to-15 ℃ at a speed of 10-20 ℃/min, freezing for 30-45 min, and removing water in the colloid to obtain a frozen material;
s2.2: the temperature in the freeze drying box is regulated to be-10-0 ℃, and the frozen materials are ground for 1-2 hours by a grinding device of the freeze drying box to obtain powdery materials;
s2.3: the powdery material is sent into a feeder through a conveyor belt, the feeder is then put into a calciner, and the mixture is calcined for 3 to 5 hours at the temperature of 1000 to 1500 ℃ and cooled to room temperature, so as to obtain an intermediate A.
Further, the doped BaTiO of step S3 3 Ball milling, specifically comprising the following steps:
s3.1: adding the intermediate A and absolute ethyl alcohol into a ball mill together, and ball milling for 0.5-1 h at a speed of 500-600 rpm;
s3.2: according to BaTiO 3 And the mass ratio of the intermediate A is 10-13:1, and BaTiO is prepared 3 Adding the mixture into a ball mill, adjusting the speed of the ball mill to be 1000-1200 rpm, and continuing ball milling for 2-3 hours to obtain mixed slurry;
s3.3: and (3) placing the mixed slurry in a dryer for drying, then grinding by a grinder, and finally sieving by a 100-200 mesh sieve to obtain an intermediate B.
Further, the step S4 of adding a binder and sintering specifically includes the following steps:
s4.1: adding the intermediate B into an airflow mixer, adding a binder, and uniformly mixing the two to obtain an intermediate C;
s4.2: adding the intermediate C into a forming press, pressing into a wafer, and then performing cold isostatic pressing to obtain an intermediate D;
s4.3: and (3) putting the intermediate D into a sintering furnace, sintering for 2-3 hours at the temperature of 1200-1500 ℃, and naturally cooling to obtain the NTC thermistor material based on the rare earth elements.
Further, the oxygen generated when nitric acid dissolves the metal oxide in the step S1.1 is dried by sodium hydroxide solid, and then collected to obtain dry oxygen, and then the dry oxygen is introduced into the sintering furnace in the step S4.3 to participate in the sintering process of the intermediate D.
Further, the rare earth oxide includes one of oxides of lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), yttrium (Y), and scandium (Sc).
Further, the binder is glue made of polyvinyl alcohol.
Further, a rare earth element-based NTC thermistor material is prepared by the preparation method of the rare earth element-based NTC thermistor material.
Compared with the prior art, the invention has the advantages that:
1. according to the invention, baTiO3 with stable high-temperature structure and good thermal sensitivity is doped for ball milling, so that the prepared NTC thermistor has stable phase structure at high temperature and has the function of measuring temperature in a high-temperature wide-temperature area, the applicability of the NTC thermistor is effectively widened, and the measurement accuracy is ensured.
2. According to the invention, the rare earth oxide is doped into the raw material of the NTC thermistor, and the rare earth oxide has better thermal stability, so that the prepared NTC thermistor material based on the rare earth element has higher resistivity and stability.
3. According to the invention, the oxygen generated by the reaction of nitric acid and metal oxide is collected and then is introduced into the sintering furnace, and sintering is assisted by using the oxygen, so that the sintering time is effectively shortened, and the effect of saving manpower and material resources is achieved.
Drawings
Fig. 1 is a flowchart of a preparation method of an NTC thermistor material based on rare earth elements according to an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
A preparation method of an NTC thermistor material based on rare earth elements, as shown in figure 1, comprises the following steps:
s1: dissolution of metal oxides with nitric acid
Adding magnesium oxide, manganese dioxide, nickel sesquioxide, ferric oxide and rare earth oxide into a reaction box containing nitric acid solution according to the mass ratio of 5:15:17:7:2, stirring and dissolving by using a stirrer to obtain nitrate solution, collecting oxygen generated by reaction by using a collecting bottle on the reaction box, wherein a filter screen containing sodium hydroxide solid is arranged at the bottle mouth of the collecting bottle for drying the oxygen, then filling absolute ethyl alcohol produced by Shanghai Colon chemical company into the stirrer, introducing the absolute ethyl alcohol into the nitrate solution from a one-way through hole on a stirring rod while stirring, pressing triethanolamine produced by Nanjing BaoGarui chemical company into the reaction box from a small hole on the inner wall of the reaction box by using a hydraulic pump after the absolute ethyl alcohol and the nitrate solution are uniformly mixed, stirring for 3 hours at the speed of 300r/min, detecting the pH value in the box in real time by using a pH detector, stopping adding the triethanolamine until the pH value in the box is 7, standing for 2 hours, and obtaining a colloid, and preparing a rare earth oxide into a NTC thermistor based on rare earth element with high thermal stability;
s2: freeze-dried jelly
Placing the colloid in a freeze drying box, cooling to-25 ℃ at a speed of 10 ℃/min, freezing for 30min, removing water in the colloid to obtain frozen materials, regulating the temperature in the freeze drying box to-10 ℃, grinding the frozen materials for 1h by a grinding device of the freeze drying box to obtain powdery materials, conveying the powdery materials into a feeder by a conveyor belt, putting the feeder into a calciner, calcining for 3h at the temperature of 1000 ℃, and cooling to room temperature to obtain an intermediate A;
s3: doped BaTiO 3 Ball milling
Adding the intermediate A and absolute ethyl alcohol produced by Changshachengning chemical engineering Co., ltd into ball mill, ball milling at 500rpm for 0.5h, and then pressing BaTiO 3 And the mass ratio of the intermediate A is 10:1, and BaTiO is added into the mixture 3 Adding into a ball mill, adjusting the speed of the ball mill to 1000rpm, continuously ball-milling for 2 hours to obtain mixed slurry, drying the mixed slurry in a dryer, grinding by a grinder, and finally sieving with a 200-mesh sieve to obtain an intermediate B, and doping BaTiO with stable high-temperature structure and good heat sensitivity 3 Ball milling is carried out, so that the prepared NTC thermistor has stable phase structure at high temperature, has the function of measuring temperature in a high-temperature wide temperature area, effectively widens the applicability of the NTC thermistor, and ensures the measurement accuracy;
s4: adding binder and sintering
Adding the intermediate B into an airflow mixer, adding a binder, uniformly mixing the two to obtain an intermediate C, adding the intermediate C into a forming press, pressing into a wafer, performing cold isostatic pressing to obtain an intermediate D, finally, placing the intermediate D into a sintering furnace, sintering at 1200 ℃ for 2 hours, introducing oxygen collected in a collecting bottle in the step S1 during sintering, and performing sintering, so that sintering time is shortened, an effect of saving manpower and material resources is achieved, and then, naturally cooling to obtain the NTC thermistor material based on the rare earth elements.
Example 2
A preparation method of an NTC thermistor material based on rare earth elements, as shown in figure 1, comprises the following steps:
s1: dissolution of metal oxides with nitric acid
Adding magnesium oxide, manganese dioxide, nickel sesquioxide, ferric oxide and rare earth oxide into a reaction box containing nitric acid solution according to the mass ratio of 7:20:25:10:3, stirring and dissolving by using a stirrer to obtain nitrate solution, collecting oxygen generated by reaction by using a collecting bottle on the reaction box, wherein a filter screen containing sodium hydroxide solid is arranged at the bottle mouth of the collecting bottle for drying the oxygen, then filling absolute ethyl alcohol produced by Shanghai Colon chemical company into the stirrer, introducing the absolute ethyl alcohol into the nitrate solution from a one-way through hole on a stirring rod while stirring, pressing triethanolamine produced by Nanjing BaoGarui chemical company into the reaction box from a small hole on the inner wall of the reaction box by using a hydraulic pump after the absolute ethyl alcohol and the nitrate solution are uniformly mixed, stirring for 3 hours at the speed of 500r/min, detecting the pH value in the box in real time by using a pH detector, stopping adding the triethanolamine until the pH value in the box is 7, standing for 2 hours, and obtaining a colloid, and preparing a rare earth oxide into a NTC thermistor based on rare earth element with high thermal stability;
s2: freeze-dried jelly
Placing the colloid in a freeze drying box, cooling to-15 ℃ at a speed of 20 ℃/min, freezing for 30min, removing water in the colloid to obtain frozen materials, regulating the temperature in the freeze drying box to-5 ℃, grinding the frozen materials for 1h by a grinding device of the freeze drying box to obtain powdery materials, conveying the powdery materials into a feeder by a conveyor belt, putting the feeder into a calciner, calcining for 3h at a temperature of 1300 ℃, and cooling to room temperature to obtain an intermediate A;
s3: doped BaTiO 3 Ball milling
Adding the intermediate A and absolute ethyl alcohol produced by Changshachengning chemical engineering Co., ltd into ball mill, ball milling at 600rpm for 0.5h, and then pressing BaTiO 3 And the mass ratio of the intermediate A is 13:1, and BaTiO is added to the mixture 3 Adding into a ball mill, adjusting the speed of the ball mill to 1200rpm, continuously ball-milling for 2 hours to obtain mixed slurry, drying the mixed slurry in a dryer, grinding by a grinder, and finally sieving with a 200-mesh sieve to obtain an intermediate B, and doping BaTiO with stable high-temperature structure and good heat sensitivity 3 Ball milling is carried out to ensure that the prepared NTC thermistor has stable phase structure at high temperature and high temperatureThe temperature measuring function of the temperature wide temperature area effectively widens the applicability of the NTC thermistor, thereby ensuring the measuring precision thereof;
s4: adding binder and sintering
Adding the intermediate B into an airflow mixer, adding a binder, uniformly mixing the two to obtain an intermediate C, adding the intermediate C into a forming press, pressing into a wafer, performing cold isostatic pressing to obtain an intermediate D, finally, placing the intermediate D into a sintering furnace, sintering at 1500 ℃ for 2 hours, introducing oxygen collected in a collecting bottle in the step S1 during sintering, and performing sintering, so that sintering time is shortened, an effect of saving manpower and material resources is achieved, and then, naturally cooling to obtain the NTC thermistor material based on the rare earth elements.
Example 3
A preparation method of an NTC thermistor material based on rare earth elements, as shown in figure 1, comprises the following steps:
s1: dissolution of metal oxides with nitric acid
Adding magnesium oxide, manganese dioxide, nickel sesquioxide, ferric oxide and rare earth oxide into a reaction box containing nitric acid solution according to the mass ratio of 5:15:17:7:2, stirring and dissolving by using a stirrer to obtain nitrate solution, collecting oxygen generated by reaction by using a collecting bottle on the reaction box, wherein a filter screen containing sodium hydroxide solid is arranged at the bottle mouth of the collecting bottle for drying the oxygen, then filling absolute ethyl alcohol produced by Shanghai Colon chemical company into the stirrer, introducing the absolute ethyl alcohol into the nitrate solution from a one-way through hole on a stirring rod while stirring, pressing triethanolamine produced by Nanjing BaoGarui chemical company into the reaction box from a small hole on the inner wall of the reaction box by using a hydraulic pump after the absolute ethyl alcohol and the nitrate solution are uniformly mixed, stirring for 5 hours at the speed of 300r/min, detecting the pH value in the box in real time by using a pH detector, stopping adding the triethanolamine until the pH value in the box is 7, standing for 3 hours, and obtaining colloid, and preparing rare earth oxide into NTC thermistor materials with higher thermal stability due to rare earth oxide;
s2: freeze-dried jelly
Placing the colloid in a freeze drying box, cooling to-25 ℃ at a speed of 10 ℃/min, freezing for 45min, removing water in the colloid to obtain frozen materials, regulating the temperature in the freeze drying box to-10 ℃, grinding the frozen materials for 2h through a grinding device of the freeze drying box to obtain powdery materials, conveying the powdery materials into a feeder through a conveying belt, putting the feeder into a calciner, calcining for 5h at a temperature of 1000 ℃, and cooling to room temperature to obtain an intermediate A;
s3: doped BaTiO 3 Ball milling
Adding the intermediate A and absolute ethyl alcohol produced by Changshachengning chemical engineering Co., ltd into ball mill, ball milling at 500rpm for 1 hr, and then pressing with BaTiO 3 And the mass ratio of the intermediate A is 10:1, and BaTiO is added into the mixture 3 Adding into a ball mill, adjusting the speed of the ball mill to 1000rpm, continuously ball-milling for 2 hours to obtain mixed slurry, drying the mixed slurry in a dryer, grinding by a grinder, and finally sieving with a 100-mesh sieve to obtain an intermediate B, and doping BaTiO with stable high-temperature structure and good heat sensitivity 3 Ball milling is carried out, so that the prepared NTC thermistor has stable phase structure at high temperature, has the function of measuring temperature in a high-temperature wide temperature area, effectively widens the applicability of the NTC thermistor, and ensures the measurement accuracy;
s4: adding binder and sintering
Adding the intermediate B into an airflow mixer, adding a binder, uniformly mixing the two to obtain an intermediate C, adding the intermediate C into a forming press, pressing into a wafer, performing cold isostatic pressing to obtain an intermediate D, finally, placing the intermediate D into a sintering furnace, sintering at 1200 ℃ for 3 hours, introducing oxygen collected in a collecting bottle in the step S1 during sintering, and performing sintering, so that sintering time is shortened, an effect of saving manpower and material resources is achieved, and then, naturally cooling to obtain the NTC thermistor material based on the rare earth elements.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (7)
1. The preparation method of the NTC thermistor material based on the rare earth elements is characterized by comprising the following steps of:
s1: dissolution of metal oxides with nitric acid
Adding magnesium oxide, manganese dioxide, nickel sesquioxide, ferric oxide and rare earth oxide into a nitric acid solution, stirring and dissolving, adding an ethanol solution, stirring and mixing, adding triethanolamine to adjust pH, stirring, and standing to obtain a colloid;
s2: freeze-dried jelly
Freeze-drying the colloid, grinding, uniformly dispersing, calcining, and cooling to room temperature to obtain an intermediate A;
s3: doped BaTiO 3 Ball milling
Adding absolute ethyl alcohol into the intermediate A, ball milling, and then adding BaTiO 3 Continuing ball milling, and then drying, grinding and sieving to obtain an intermediate B;
s4: adding binder and sintering
Adding a binder into the intermediate B, uniformly mixing, pressing into a wafer, performing high-temperature sintering, and naturally cooling to obtain the NTC thermistor material based on the rare earth elements;
the step S1 of dissolving the metal oxide by nitric acid specifically comprises the following steps:
s1.1: adding magnesium oxide, manganese dioxide, nickel sesquioxide, ferric oxide and rare earth oxide into a reaction box containing nitric acid solution according to the mass ratio of 5-7:15-22:17-25:5-10:2-3, and stirring and dissolving by using a stirrer to obtain nitrate solution;
s1.2: filling absolute ethyl alcohol into a stirrer, and introducing the absolute ethyl alcohol into the nitrate solution from a one-way through hole on a stirring rod while stirring by the stirrer;
s1.3: after the absolute ethyl alcohol and the nitrate solution are uniformly mixed, the triethanolamine is pressed into the reaction box from the small holes on the inner wall of the reaction box through a hydraulic pump, and is stirred for 3 to 5 hours at the speed of 300 to 500 r/min;
s1.4: the pH value in the reaction box is detected in real time by a pH detector in the reaction box, the addition of triethanolamine is stopped until the pH value in the box is=6-7, the stirring is stopped, and the reaction box is kept stand for 2-3 hours to obtain a colloid;
the doped BaTiO of the step S3 3 Ball milling, specifically comprising the following steps:
s3.1: adding the intermediate A and absolute ethyl alcohol into a ball mill together, and ball milling for 0.5-1 h at a speed of 500-600 rpm;
s3.2: according to BaTiO 3 And the mass ratio of the intermediate A is 10-13:1, and BaTiO is prepared 3 Adding the mixture into a ball mill, adjusting the speed of the ball mill to be 1000-1200 rpm, and continuing ball milling for 2-3 hours to obtain mixed slurry;
s3.3: and (3) placing the mixed slurry in a dryer for drying, then grinding by a grinder, and finally sieving by a 100-200 mesh sieve to obtain an intermediate B.
2. The method for preparing an NTC thermistor material based on rare earth elements according to claim 1, wherein the freeze-dried gel of step S2 comprises the following steps:
s2.1: placing the colloid in a freeze drying box, cooling to-25 to-15 ℃ at a speed of 10-20 ℃/min, freezing for 30-45 min, and removing water in the colloid to obtain a frozen material;
s2.2: the temperature in the freeze drying box is regulated to be-10-0 ℃, and the frozen materials are ground for 1-2 hours by a grinding device of the freeze drying box to obtain powdery materials;
s2.3: the powdery material is sent into a feeder through a conveyor belt, the feeder is then put into a calciner, and the mixture is calcined for 3 to 5 hours at the temperature of 1000 to 1500 ℃ and cooled to room temperature, so as to obtain an intermediate A.
3. The method for preparing the NTC thermistor material based on rare earth element according to claim 2, wherein the binder is added and sintered in the step S4, specifically comprising the steps of:
s4.1: adding the intermediate B into an airflow mixer, adding a binder, and uniformly mixing the two to obtain an intermediate C;
s4.2: adding the intermediate C into a forming press, pressing into a wafer, and then performing cold isostatic pressing to obtain an intermediate D;
s4.3: and (3) putting the intermediate D into a sintering furnace, sintering for 2-3 hours at the temperature of 1200-1500 ℃, and naturally cooling to obtain the NTC thermistor material based on the rare earth elements.
4. The method of claim 3, wherein the oxygen generated when nitric acid dissolves the metal oxide in step S1.1 is dried by sodium hydroxide solid, and then collected to obtain dry oxygen, and the dry oxygen is introduced into the sintering furnace in step S4.3 to participate in the sintering process of the intermediate D.
5. The method of claim 1, wherein the rare earth oxide comprises one of oxides of lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), yttrium (Y), and scandium (Sc).
6. The method for preparing a rare earth element-based NTC thermistor material according to claim 3, wherein the binder is glue made of polyvinyl alcohol.
7. An NTC thermistor material based on rare earth elements, characterized in that it is prepared by a preparation method of an NTC thermistor material based on rare earth elements as claimed in any one of claims 1 to 6.
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