CN111128495A - NTC thermistor element for high-temperature measurement and manufacturing method thereof - Google Patents
NTC thermistor element for high-temperature measurement and manufacturing method thereof Download PDFInfo
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- H01C7/04—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient
- H01C7/041—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient formed as one or more layers or coatings
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses an NTC thermistor element for high-temperature measurement and a manufacturing method thereof. The NTC thermistor element for high-temperature measurement solves the problem that the negative temperature coefficient thermistor cannot be used in a high-temperature environment.
Description
Technical Field
The invention belongs to the field of electronic element manufacturing, and particularly relates to an NTC thermistor element for high-temperature measurement and a manufacturing method thereof.
Background
A conventional negative temperature coefficient thermistor (NTC) is manufactured by doping two or more transition metal oxides such as cobalt oxide, manganese oxide, nickel oxide, iron oxide, copper oxide and aluminum oxide through a tape casting or dry pressing forming mode to prepare slurry or powder, forming, sintering and electrode manufacturing are adopted to prepare an NTC thermistor chip, and then processes such as welding, encapsulation or glass packaging are adopted to prepare the NTC thermistor, the NTC thermistor is widely applied within the temperature range of-50-350 ℃, but the NTC thermistor of the type exceeding 350 ℃ cannot be reliably used.
Disclosure of Invention
In view of the drawbacks of the prior art thermistor devices, the present invention has developed a new NTC thermistor device. The NTC thermistor element adopts a novel structure, and the lead part is directly contacted with the chip part, so that the reliability reduction caused by the thermolabile part in the use process is avoided.
Specifically, the invention adopts the following technical scheme:
an NTC thermistor element for high-temperature measurement comprises a chip and a lead wire, and is characterized in that the lead wire is directly embedded in the chip and is in direct contact with chip materials, wherein the chip is formed by bonding chip slurry on the lead wire and then firing the chip slurry, and the lead wire is a high-temperature-resistant metal lead wire. Wherein the chip is prepared by bonding chip slurry prepared from metal oxide mixture and binder on lead wire, and firing, wherein the metal oxide is prepared from oxides or minerals of manganese, cobalt, nickel, iron, copper, aluminum, yttrium, zirconium, etc. at a certain ratio, such as SiO2、CuO、Mn3O4、NiO、Fe2O3、Al2O3、Co3O4Combinations of any of the above. In the chip paste, a binder is included or not included, and in a preferred embodiment, the binder is a water-soluble binder, such as polyvinyl alcohol, starch, dextrin, carboxymethyl cellulose, and the like. The binder may be added to the slurry as a dry powder or as an aqueous solution, for example polyvinyl alcohol added to the slurry as a dry powder or as an aqueous solution. In a preferred embodiment, a dispersant is further included, such as polyacrylamide, sodium polyacrylate, sodium hexametaphosphate, sodium pyrophosphate, and the like, and in a more preferred embodiment, the dispersant is polyacrylamide. Preferably, the lead wire is a platinum lead wire.
The present invention further discloses a method for manufacturing an NTC thermistor device for pyrometry, characterized in that the method comprises the steps of: 1) preparing chip slurry: weighing metal oxide in proportion, grinding to required fineness, and preparing into slurry with water content of 30-50%; 2) preparing a lead: arranging the leads in a group of two leads at a required interval, and reserving enough length of the leads for inserting into the chip slurry; 3) preparing a lead chip slurry combination: inserting the leads into the chip slurry to a required depth and maintaining for a sufficient time, then lifting the leads to wrap sufficient chip slurry on each group of leads, and drying to form a lead chip slurry combination body; 4) and (3) sintering: and (3) feeding the dried lead chip slurry combination into a sintering furnace for sintering to obtain the NTC thermistor element for high-temperature measurement.
In the method of the invention, the chip slurry is prepared by grinding a mixture of metal oxide and grinding fluid in a mill, wherein the ratio of the metal oxide to the grinding fluid is 1: 0.7-1.0. Wherein the grinding liquid is water or ethanol water solution with the concentration of 5-20%.
Preferably, the slurry obtained after the primary grinding is dried, and then the grinding fluid is added for secondary grinding to a desired fineness. Further preferably, the method further comprises, after drying and before secondary grinding, pre-burning the dried powder in a pre-burning furnace, and then performing secondary grinding. When the pre-firing is performed, the pre-firing temperature is preferably 850 ℃ 15 ℃ and the pre-firing time is preferably 2. + -. 0.2 hours.
In a preferred embodiment, the slurry is discharged after grinding, and preferably the slurry further comprises a step of adding a binder and a dispersant, and the slurry is discharged after grinding again after adding the binder and the dispersant. In a more preferred embodiment, the slurry is discharged after grinding after adding the polyvinyl alcohol binder in an amount of 0-3% by weight of the powder and the polyacrylamide dispersant in an amount of 0.2-0.6% by weight of the powder, and is discharged after grinding again.
In the method of the present invention, it is preferable that the chip is not formed at one time, but the step 3) is repeated a plurality of times to obtain a suitable chip size, wherein the step 3) is repeated a plurality of times to stick the core piece slurry again on the lead chip slurry combination formed after drying and to dry again, thereby enlarging the size of the lead chip slurry combination, and is repeated a sufficient number of times until the formed lead chip slurry combination reaches a sufficient size.
In the method of the present invention, the sintering temperature in step 4) is 1000-.
In the manufacturing of the element, the chip is in direct contact with the lead, and the lead forms a preformed body of the chip at the front end of the lead in a manner of sticking core sheet slurry, so that the manufactured lead is embedded in the chip, the full combination of the chip and the lead is ensured, and the combination strength is improved. Due to the structure, silver paste does not need to be welded, the using environment is not affected by the temperature of welding and soldering flux, and the self performance of the silver paste is not limited, so that the obtained element can adapt to higher using temperature.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of the present invention;
fig. 2 is a perspective structural diagram of the element of the present invention.
In the figure: 1. ceramic material; 2. and (7) leading wires. Wherein L is the lead pitch and A is the lead buried depth.
Detailed Description
The invention provides a novel manufacturing method of an NTC thermistor element for high-temperature measurement and a resistor element manufactured by the method. In the existing thermistor manufacturing method, metal oxides are weighed in proportion and ground to prepare slurry, then the slurry is preformed and fired to prepare a chip, then a lead is welded on the chip, and then the chip is encapsulated. The resistance element manufactured by the conventional manufacturing method can endure a high temperature below 350 c due to the properties of the solder and the encapsulant itself, but when the usage environment exceeds 350 c, the performance of the element becomes unreliable.
In view of the above, the present invention provides a new method for manufacturing a thermistor device. In the method of the invention, the process of manufacturing a formed chip in advance in the traditional method is changed, the chip slurry is directly formed with the lead, and then the element is directly fired.
As shown in fig. 1, when a preform of a chip is formed on a platinum wire lead by dip bonding, the bonding between the chip paste and the lead is more tight and firm, and after sintering, the chip paste is vitrified to form a ceramic material, which is sufficiently bonded to the lead, and thus the performance of the resistor element is more easily exhibited.
As further shown in fig. 2, the resistance range and the resistance accuracy of the core element of the conventional negative temperature coefficient thermistor are related to the thickness of the chip and the electrode area, and the resistance range and the resistance accuracy of the core element of the thermistor adopting the structure of the invention are related to the lead pitch size (fig. L value) of the two platinum wires and the length size (fig. a value) of the platinum wire immersed in the ceramic body.
The invention provides an NTC thermistor element for high-temperature measurement, which comprises a chip and a lead wire, wherein the lead wire is directly embedded in the chip and is in direct contact with chip materials, the chip is formed by bonding chip slurry on the lead wire and then firing the chip slurry, and the lead wire is a high-temperature-resistant metal lead wire. The chip is prepared by bonding chip slurry prepared from a metal oxide mixture and a binder on a lead wire and then firing, wherein the chip slurry is prepared by grinding metal oxides after being prepared in proportion, and the metal oxides are prepared from oxides or minerals of manganese, cobalt, nickel, iron, copper, aluminum, yttrium, zirconium and other metals in a certain proportion, such as SiO2、CuO、Mn3O4、NiO、Fe2O3、Al2O3、Co3O4Combinations of any of the above. The high temperature resistant lead wire comprises various suitable metal or metal alloy and lead wires made of non-metal conductive materials, such as: metal lead wires of platinum, rhodium, tungsten, tantalum, niobium, etc., metal alloy lead wires of iron-chromium-aluminum-magnesium alloy, nickel-chromium alloy, etc., lead wires of carbon fiber, etc., ZnO doped with Al2O3In a preferred embodiment, the lead wire is a platinum lead wire.
The present invention further discloses a method for manufacturing an NTC thermistor device for pyrometry, the method comprising the steps of: 1) preparing chip slurry: weighing metal oxide in proportion, grinding to required fineness, and preparing into slurry with water content of 40-50%; 2) preparing a lead: arranging the leads in a group of two leads at a required interval, and reserving enough length of the leads for inserting into the chip slurry; 3) preparing a lead chip slurry combination: inserting the leads into the chip slurry to a required depth and maintaining for a sufficient time, then lifting the leads to wrap sufficient chip slurry on each group of leads, and drying to form a lead chip slurry combination body; 4) and (3) sintering: and (3) feeding the dried lead chip slurry combination into a sintering furnace for sintering to obtain the NTC thermistor element for high-temperature measurement.
In the method of the invention, the chip slurry is prepared by grinding a mixture of metal oxide and grinding fluid in a mill, wherein the ratio of the metal oxide to the grinding fluid is 1: 0.7-1.0. Wherein the grinding fluid is water or a process control agent is added thereto, water can also be regarded as one of the process control agents, but in the method of the present invention, the end point is not only to obtain particles of the metal mixture, but more importantly to obtain a slurry having a suitable viscosity and a uniform distribution of the particles of the metal mixture, and water is an important constituent of the slurry. The process control agent is typically an alcohol, ester, or like compound, such as ethanol, propanol, propylene glycol, stearic acid, or the like. In a preferred embodiment of the invention, and in accordance with the object of the invention, the process control agent used is an aqueous ethanol solution having a concentration of 5 to 20%, which is effective in promoting a uniform distribution of the particles in the slurry mixture during the milling process.
Preferably, the slurry obtained after the primary grinding is dried, and then the grinding fluid is added for secondary grinding to a desired fineness. Further preferably, before the secondary grinding after the drying, the method further comprises the steps of pre-sintering the powder obtained after the drying in a pre-sintering furnace, and then performing the secondary grinding, so that the processes of curing, destroying and reconstructing the particle structure of the powder are performed, the pre-synthesis, homogenization and activation of the powder particles are realized, and the more excellent electrical properties of the final product are realized. When the pre-firing is performed, the pre-firing temperature is preferably 850 ℃ 15 ℃ and the pre-firing time is preferably 2. + -. 0.2 hours.
In a preferred embodiment, a binder and a dispersant are also added to the finally obtained slurry, and the binder and the dispersant are preferably added after grinding the slurry and before discharging, namely, the binder and the dispersant are added to the mill before discharging and are mixed in the slurry by the operation of the mill again or are added during the operation of the mill. Therefore, the method of the present invention preferably further comprises the steps of: adding polyvinyl alcohol adhesive and polyacrylamide dispersant in 0-3 wt% of the powder material, grinding again and discharging. The choice of binder can be varied and the preferred solution is polyvinyl alcohol, taking into account the effect on the viscosity of the final chip slurry and the elimination of the effect on the properties of the final product during the process. The choice of the dispersant can be various, and the preferable scheme is polyacrylamide which is an organic high polymer material in consideration of the influence of various dispersants on the chip slurry.
In the method of the present invention, it is preferable that the chip is not formed at one time, but the step 3) is repeated a plurality of times to obtain a suitable chip size, wherein the step 3) is repeated a plurality of times to stick the core piece slurry again on the lead chip slurry combination formed after drying and to dry again, thereby enlarging the size of the lead chip slurry combination, and is repeated a sufficient number of times until the formed lead chip slurry combination reaches a sufficient size. The multiple molding is beneficial to forming a favorable internal structure of the chip preforming body, reduces stress, and reduces the influence of the change of the chip on the firmness of the combination of the chip and the lead during sintering. However, the number of times of the dipping is too large to control the manufacturing process of the chip preform and to lower the production efficiency, so that the number of times of the dipping can be controlled by adjusting the amount of the polyvinyl alcohol added. In a preferred embodiment, the dipping times are controlled to be 2-10 times, the addition amount of the adhesive polyvinyl alcohol is about 2% by weight of the raw powder, and the addition amount of the dispersant polyacrylamide is about 0.3% by weight of the raw powder.
In the method of the present invention, the sintering temperature in step 4) is 1000-.
The negative temperature coefficient thermistor is characterized in that a ceramic material is stuck on two parallel platinum wire leads in a dipping and sticking mode, and the dipping and sticking depths of the platinum wire leads are required to be consistent. The thermistor is characterized in that the whole negative temperature coefficient thermistor is formed by sintering at the temperature of 1000-1400 ℃, can be used in the environment with the temperature of 900 ℃, and solves the problem that the negative temperature coefficient thermistor cannot be used in the high-temperature environment.
The invention is further illustrated by the following examples.
Preparation of chip slurry
The chip slurry is prepared by mixing metal oxides (manganese, cobalt, nickel, iron, copper, aluminum, yttrium, zirconium and the like) according to a certain proportion, grinding for the first time, drying, pre-sintering, grinding for the second time and adding a binder according to a certain proportion, and the specific process comprises the following steps:
1. preparing materials: the raw materials are prepared according to a certain molar ratio;
2. primary grinding: grinding the prepared metal oxide powder in a planetary ball mill according to a certain material-ball ratio to obtain a primary grinding material;
3. drying: pouring the primary grinding material into a stainless steel disc, and placing the stainless steel disc in an oven for drying;
4. pre-burning: sieving the dried powder with a stainless steel sieve of 20 meshes, crushing, pouring into a high-temperature resistant porcelain dish, putting into a presintering furnace for presintering at the presintering temperature of 850 +/-15 ℃, and preserving heat for 2 hours, wherein the cooling mode is furnace natural cooling;
5. and (3) secondary grinding: grinding the pre-sintered powder in the same way as the first grinding;
6. adding a binder and a dispersant: adding a polyvinyl alcohol adhesive and a polyacrylamide dispersing agent into the mill before secondary grinding and discharging according to requirements, grinding for 30 minutes, and discharging.
Secondly, lead wire dipping and sticking
1. Preparing a lead: arranging the leads on the tooling plate, wherein every two leads form a group, the interval between the two leads is 1-3 mm, and one end of each lead is tidily arranged to ensure the consistency of dipping and sticking;
2. tape pasting: adhering an adhesive tape on the tooling plate, fixing the lead on the tooling plate and ensuring that one end of the lead is exposed to a sufficient length;
3. dipping and sticking: and immersing the exposed ends of the leads in the chip slurry for 1-3 mm, keeping for 1-2 seconds, taking out, drying, and repeating the process for 3-5 times to obtain a chip preform with the width of about 3-5 mm and the thickness of about 2-3 mm.
Thirdly, sintering
And transferring the obtained chip preformed body to a sintering tool, and sintering in a sintering furnace at the sintering temperature of 1000-1400 ℃ for 2 +/-0.2 hours to obtain the high-temperature-resistant thermistor element.
Example 1
The method comprises the steps of preparing materials according to a molar ratio of Mn to Ni to Al =40 to 50 to 10, feeding and grinding the materials into a planetary ball mill at a speed of V = 200-220 rpm at a ball to water =1 to 4 to 0.9 mass ratio, rotating the materials forwards and backwards every 30 minutes, grinding the materials for 8 hours, and discharging the materials. Pouring the slurry into a stainless steel plate, placing the stainless steel plate into an oven, and drying the stainless steel plate at the temperature of 80 +/-10 ℃ for 12 +/-1 hour. Sieving the dried powder with a stainless steel sieve of 20 meshes, crushing, pouring into a high-temperature resistant porcelain dish, putting into a pre-sintering furnace for pre-sintering, wherein the pre-sintering temperature is as follows: keeping the temperature for 2 +/-0.2 hours at 850 +/-15 ℃, turning off the power supply after the temperature is up to the temperature, and taking out the product after the temperature is naturally cooled to 40-60 ℃. And (3) grinding the pre-sintered powder again for the second time in the same grinding mode as the first grinding mode, and discharging no material after grinding. Adding polyvinyl alcohol adhesive and 0.3 percent polyacrylamide dispersant according to 2 percent of the weight of the original powder, grinding for 30 minutes, and discharging to obtain the slurry.
Examples 2 to 3
A slurry was prepared in the same manner as in example 1 except that water in grinding was replaced with a 5%, 20% ethanol aqueous solution, respectively.
Examples 4 to 6
Slurries were prepared in the same manner as in examples 1 to 3, except that after the secondary grinding, polyvinyl alcohol was not added, or 1% of polyvinyl alcohol was added, based on the weight of the polyvinyl alcohol dry powder in the slurry.
Examples 7 to 9
Slurries were prepared in the same manner as in examples 1 to 3, except that after the secondary grinding, polyvinyl alcohol was not added, or 3% of polyvinyl alcohol was added, based on the weight of the polyvinyl alcohol dry powder in the slurry.
Examples 10 to 18
Ingredients were formulated at a molar ratio of Mn: Co: Al =36.7:46.7:16.7, and then slurries were prepared in the same manner as in examples 1 to 9.
The slurries prepared in the manner described in examples 1-18 above were placed in appropriate amounts in slurry tanks that were formed as shallow, elongated channels having a length similar to the tooling plates used to arrange the leads. The platinum lead wires are well arranged on the tooling plate, and are soaked and adhered in a slurry tank after the adhesive tape is adhered. Multiple sets of leads were prepared for comparison of different tack-free times, which were divided into 1 second, 2 seconds, 3 seconds, and 5 seconds. And (5) soaking and bonding each group of leads for 5 times according to the soaking and bonding procedure, and observing the form of the obtained chip preformed body.
And sintering the obtained pre-formed body in a sintering furnace at the sintering temperature of 1000-1400 ℃ for 2 +/-0.2 hours to obtain the NTC thermistor element for high-temperature measurement, and detecting.
While the embodiments of the present invention have been described in detail with reference to the drawings and the specific examples, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (10)
1. An NTC thermistor element for high-temperature measurement comprises a chip and a lead wire, and is characterized in that the lead wire is directly embedded in the chip and is in direct contact with chip materials, wherein the chip is formed by bonding chip slurry on the lead wire and then firing the chip slurry, and the lead wire is a high-temperature-resistant metal lead wire.
2. A method of manufacturing an NTC thermistor element for pyrometry, the method comprising the steps of: 1) preparing chip slurry: weighing metal oxide in proportion, grinding to required fineness, and preparing into slurry with water content of 30-50%; 2) preparing a lead: arranging the leads in a group of two leads at a required interval, and reserving enough length of the leads for inserting into the chip slurry; 3) preparing a lead chip slurry combination: inserting the leads into the chip slurry to a required depth and maintaining for a sufficient time, then lifting the leads to wrap sufficient chip slurry on each group of leads, and drying to form a lead chip slurry combination body; 4) and (3) sintering: and (3) feeding the dried lead chip slurry combination into a sintering furnace for sintering to obtain the NTC thermistor element for high-temperature measurement.
3. The method of manufacturing an NTC thermistor device for pyrometry according to claim 2, wherein the chip slurry is ground from a mixture of a metal oxide and a grinding liquid in a mill in which the ratio of the metal oxide to the grinding liquid is 1:0.7 to 1.0.
4. The method of manufacturing an NTC thermistor device for pyrometry according to claim 3, wherein the abrasive liquid is water or an aqueous solution of ethanol having a concentration of 5 to 20%.
5. The method of manufacturing an NTC thermistor device for high temperature measurement according to claim 3, wherein the slurry obtained after the primary grinding is dried, and then the secondary grinding is performed with a grinding fluid to a desired fineness.
6. The method of manufacturing an NTC thermistor element for pyrometry according to claim 5, further comprising: and pre-burning the powder obtained after drying in a pre-burning furnace before secondary grinding after drying, and then carrying out secondary grinding.
7. The method of manufacturing an NTC thermistor device for pyrometry according to claim 6, wherein the pre-firing temperature is 850 ℃ ± 15 ℃, and the pre-firing time is 2 ± 0.2 hours.
8. The method of manufacturing an NTC thermistor element for pyrometry according to claim 3 or 5, further comprising: before discharging, adding the adhesive and the dispersing agent, and discharging after grinding again.
9. The method of manufacturing an NTC thermistor device for pyrometry according to claim 2, wherein the step 3) is repeated to stick the chip paste again on the wire-chip-paste combination formed after drying and to dry again, thereby enlarging the size of the wire-chip-paste combination, and is repeated a sufficient number of times until the formed wire-chip-paste combination reaches a sufficient size.
10. The method of manufacturing an NTC thermistor device for pyrometry according to claim 2, characterized in that the sintering temperature is 1000-1400 ℃.
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| CN109053158A (en) * | 2018-08-28 | 2018-12-21 | 深圳市汇北川电子技术有限公司 | Thermal sensitive ceramic powder, NTC heat sensitive chip, temperature sensor and preparation method |
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