CN1079570C - Oxide semiconductor thermal sensitive resistor and its producing method - Google Patents
Oxide semiconductor thermal sensitive resistor and its producing method Download PDFInfo
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- CN1079570C CN1079570C CN97122363A CN97122363A CN1079570C CN 1079570 C CN1079570 C CN 1079570C CN 97122363 A CN97122363 A CN 97122363A CN 97122363 A CN97122363 A CN 97122363A CN 1079570 C CN1079570 C CN 1079570C
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Abstract
The present invention relates to an oxide semi-conductor thermo-sensitive resistor and a manufacture method thereof. The present invention mainly takes nitrates or acetates of Al, Mn and Ni as raw materials, material powder is prepared by a liquid phase coprecipitation method, emulsifier OP is added for cleaning, and the powder is prepared after decomposition, grinding and presintering. The thermo-sensitive resistor is in an epoxy lead wire bead shape with sealed single end and has the characteristics of small size, high stability, high reliability, etc., and the thermo-sensitive resistor is suitable for electronic fields.
Description
The present invention relates to a kind of oxidate semi-condcutor thermo-sensitive resistance and manufacture method thereof
Oxidate semi-condcutor thermo-sensitive resistance of the present invention has little, the good stability of volume for epoxy sealing two ends lead-in wire pearl, and characteristics such as reliability height are applicable to the measurement of electrothermometer equitemperature, control and line build-out.The product of the existing same spline structure of Japan, same parameter comes out, but such device of China relies on import substantially, costs an arm and a leg.
In general, the semiconductor temperature-sensitive material of performance of the same race, because its manufacture craft difference, Main Ingredients and Appearance and ratio thereof also have than big-difference.Japan adopts nitrate heat of mixing decomposition method to prepare powder body material, and its electrical parameter is: 825/85=4013 ± 1%, R
25=83K Ω.Domestic preparation oxide heat sensitive material normally adopts oxide mixed grinding method.The present invention is through for many years exploration, research, and adopting the nitrate or the acetate of aluminium, manganese, nickel is raw material, and with liquid-phase coprecipitation powder process body, its ratio and technology have marked difference.The parameter index of products obtained therefrom all reaches external like product index.
The object of the invention is, the manufacture method of oxidate semi-condcutor thermo-sensitive resistance of development is that nitrate or the acetate with aluminium, manganese, nickel is raw material, adopt liquid-phase coprecipitation to prepare the material powder, adding polyoxyethylene nonylphenol ether cleans, then powder is decomposed, grind, presintering, carry out preforming, isostatic cool pressing, high temperature sintering again and make, its electrical parameter index of this products obtained therefrom all reaches Japanese like product level, thereby has substituted the situation of like product dependence import.
The manufacture method of oxidate semi-condcutor thermo-sensitive resistance of the present invention, it mainly is that the manufacture method of this thermistor is to analyze pure molar percentage % cobalt 3-5, manganese 80-45, the nitrate of nickel 15-52 or acetate are raw material, adopt liquid-phase coprecipitation to prepare the powder precipitated liquid, precipitated liquid is the aluminium of concentration 1N, manganese, the salting liquid of nickel, the polyoxyethylene nonylphenol ether that adds weight 1%, under violent stirring, evenly add precipitation reagent in the precipitated liquid, precipitation adds that deionized water cleans and solution is carried out sonicated after finishing repeatedly, oven dry, thermal decomposition, levigate, presintering, carry out preforming again, the isostatic cool pressing high temperature sintering is made; Must strictly control precipitated liquid and the concentration of precipitation reagent carbonic hydroammonium and the ratio of measuring between the two in operation; Precipitation reagent concentration is the ammonium bicarbonate soln of 1.5-2%, and the addition of precipitation reagent is a 2-2.5 times of volume ratio of precipitated liquid; In thermal decomposition, temperature is 400-500 ℃, time 5-10 hour; In presintering, temperature is 650-800 ℃; In preforming, carry out the isostatic cool pressing high temperature sintering after material is pre-formed as φ 50mm left and right sides cylinder, wherein the pressure of isostatic cool pressing is 2.0-3.51/cm
2, 1180-1200 ℃ of high temperature sintering 2 hours, the lifting temperature was controlled at 1-1.5 ℃/minute then; With the cylinder disk behind the sintering cut into slices, two sides blackening AgPd electrode, scribing, be the stamen sheet, and then after the stamen sheet adopted soldering technology welding lead, apply one deck PPS three anti-insulating varnish at stamen sheet and lead-in wire root earlier, adopt SWF at last
12-SB embedding epoxy packages Cheng Zhuti.
The manufacture method of oxidate semi-condcutor thermo-sensitive resistance of the present invention has original solution in the following areas:
(1) when adopting liquid-phase coprecipitation to prepare powder, too high as the pH value of solution, the sediment of some element can produce complexing and dissolve; PH value is low excessively, some element can not precipitate again fully, and pH value is a parameter that is difficult to accurately control in chemical reaction, this certainly will cause the powder element ratio and the original formulation that are settled out variant, and each technology all is difficult to repetition, and the present invention takes strict control precipitated liquid and the concentration of precipitation reagent and the ratio of measuring between the two, and precipitation reagent evenly slowly adds, the temperature of precipitated liquid is controlled in the 30-40 ℃ of scope all the time, thereby reaches the purpose of control powder element ratio.
(2) to make powder thinner because of liquid-phase coprecipitation, the powder surface activity is big, reunites further this reunion of aggravation of a large amount of anionic existence in the precipitated liquid especially easily, cause granularity big, inhomogeneous, the consistency of material is very poor, and the present invention adds emulsifying agent in precipitated liquid, reduce the surface activity of powder, add deionized water with sediment and clean repeatedly, carry out sonicated simultaneously, destroy the reunion of powder.Before pre-burning, introduce thermal decomposition process, decompose the back powder is ground.
(3) traditional quick resistance of pearl body heat or thick-film thermistor, because material behavior is inhomogeneous, temperature-sensitive stamen chip size is inconsistent, the influence of factors such as electrode effect, packaging technology causes the inconsistent of component parameters.The present invention introduces the cold isostatic compaction technology, adopts section, scribing process, has guaranteed that product has higher consistency.
(4) thermistor that adopts the present invention to produce, its stamen chip size should be at V=a * a * d, 0.70＜a＜1.00mm; 0.20 in＜d＜0.30mm scope, its electrical parameter 825/50=3950 ± 1%, R25 ℃=83 ± 3%K Ω.
Embodiment 1:
Use commercially available analysis pure by aluminum nitrate 5%, manganese nitrate 80%, nickel nitrate 15% (mol ratio) as proportion of raw material weighing 2mol, be mixed with the precipitated liquid that concentration is 1M, solution temperature is at 30-40 ℃.
Use the pure carbonic hydroammonium 6mol of commercially available analysis as precipitation reagent, be mixed with the precipitant solution that concentration is 2M, solution temperature is controlled at 30-40 ℃;
Add the emulsifier op-10 of 1% weight in precipitated liquid, and in vigorous stirring the speed of precipitation reagent by 50-100ml/ minute is evenly added, till adding, precipitation process is finished;
To have sedimentary solution and place Ultrasound Instrument to handle 10 minutes, and carry out suction filtration, and add the 3000ml deionized water again, temperature is at 30-40 ℃, stirring-sonicated-filter, and this process is 3-5 time repeatedly, dries levigate;
Powder was 400 ℃ of thermal decompositions 10 hours, and is levigate, 800 ℃ of pre-burnings 3 hours, levigate then, and the powder preparing process finishes;
Carry out isostatic cool pressing after pressed by powder being become the cylinder of Φ 50mm, pressure is 2.0-3.51/cm
2Then 1180 ℃ of sintering 2 hours, the lifting temperature is controlled at 1-1.5 ℃/minute, use slicing machine, the cylinder that sintering is intact is cut into disk, two sides blackening AgPd electrode, divide electrode stamen sheet again into, with behind the stamen sheet welding lead, apply one deck PPS three anti-insulating varnish at stamen sheet and lead-in wire root earlier again, then adopt SMF
12-SB embedding epoxy packages Cheng Zhuti.
The quick resistance electrical parameter of gained pearl body heat B25/50=3950 ± 1%, R25 ℃=83 ± 3%K Ω
Embodiment 2:
Use commercially available analysis pure by aluminum nitrate 3%, manganese nitrate 45%, nickel nitrate 52% (mol ratio) as proportion of raw material weighing 2mol, be mixed with the precipitated liquid that concentration is 1M, solution temperature is at 30 ± 2 ℃.
Use the pure carbonic hydroammonium 6mol of commercially available analysis as precipitation reagent, be mixed with the precipitant solution that concentration is 1.5M, solution temperature is controlled at 30-40 ℃;
Add the emulsifier op-10 of 1% weight in precipitated liquid, and in vigorous stirring the speed of precipitation reagent by 50-100ml/ minute is evenly added, till adding, precipitation process is finished;
To have sedimentary solution and place Ultrasound Instrument to handle 10 minutes, and carry out suction filtration, and add the 3000ml deionized water again, temperature is at 30-40 ℃, stirring-sonicated-suction filtration, and this process is 3-5 time repeatedly, dries levigate;
Powder was 500 ℃ of thermal decompositions 6 hours, and is levigate, 800 ℃ of pre-burnings 3 hours, levigate then, and the powder preparing process finishes;
Carry out isostatic cool pressing after pressed by powder being become the cylinder of Φ 50mm, pressure is 2.0-3.5l/cm
2Then 1200 ℃ of sintering 2 hours, the lifting temperature is controlled at 1-1.5 ℃/minute, use slicing machine, the cylinder that sintering is intact is cut into disk, two sides blackening AgpP electrode, divide electrode stamen sheet again into, with behind the stamen sheet welding lead, apply one deck PPS three anti-insulating varnish at stamen sheet and lead-in wire root earlier again, then adopt SMF
12-SB embedding epoxy packages Cheng Zhuti.
The quick resistance electrical parameter of gained pearl body heat B25/50=3950 ± 1%, R25 ℃=83K Ω
Embodiment 3:
Use commercially available analysis pure by aluminum nitrate 4%, manganese nitrate 66%, nickel nitrate 30% (mol ratio) as proportion of raw material weighing 2mol, be mixed with the precipitated liquid that concentration is 1M, solution temperature is at 30-40 ℃.
Use the pure carbonic hydroammonium 6mol of commercially available analysis as precipitation reagent, be mixed with the precipitant solution that concentration is 1M, solution temperature is controlled at 30-40 ℃;
Add the emulsifier op-10 of 1% weight in precipitated liquid, and in vigorous stirring the speed of precipitation reagent by 50-100ml/ minute is evenly added, till adding, precipitation process is finished;
To have sedimentary solution and place Ultrasound Instrument to handle 10 minutes, and carry out suction filtration, and add the 3000ml deionized water again, temperature is at 30-40 ℃, stirring-sonicated-suction filtration, and this process is 3-5 time repeatedly, dries levigate;
Powder was 400 ℃ of thermal decompositions 5 hours, and is levigate, 800 ℃ of pre-burnings 3 hours, levigate then, and the powder preparing process finishes;
Carry out isostatic cool pressing after pressed by powder being become the cylinder of Φ 50mm, pressure is 2.0-3.5l/cm
2Then 1180 ℃ of sintering 2 hours, the lifting temperature is controlled at 1-1.5 ℃/minute, use slicing machine, the cylinder that sintering is intact is cut into disk, two sides blackening AgPd electrode, divide electrode stamen sheet again into, with behind the stamen sheet welding lead, apply one deck PPS three anti-insulating varnish at stamen sheet and lead-in wire root earlier again, then adopt SMF
12-SB embedding epoxy packages Cheng Zhuti.
The quick resistance electrical parameter of gained pearl body heat B25/50=3950 ± 1%, R25 ℃=83K Ω
Embodiment 4:
Use commercially available analysis pure by aluminum nitrate 5%, manganese nitrate 80%, nickel nitrate 15% (mol ratio) as proportion of raw material weighing 2mol, be mixed with the precipitated liquid that concentration is 1M, solution temperature is at 30-40 ℃.
Use the pure carbonic hydroammonium 6mol of commercially available analysis as precipitation reagent, be mixed with concentration and be 2% precipitant solution, solution temperature is controlled at 30-40 ℃;
Add the emulsifier op-10 of 1% weight in precipitated liquid, and in vigorous stirring the speed of precipitation reagent by 50-100ml/ minute is evenly added, till adding, precipitation process is finished;
To have sedimentary solution and place Ultrasound Instrument to handle 10 minutes, and carry out suction filtration, and add the 3000ml deionized water again, temperature is at 30-40 ℃, stirring-sonicated-suction filtration, and this process is 3-5 time repeatedly, dries levigate;
Powder was 500 ℃ of thermal decompositions 5 hours, and is levigate, 700 ℃ of pre-burnings 3 hours, levigate then, and the powder preparing process finishes;
Carry out isostatic cool pressing after becoming the post of φ 50mm to stop the pressed by powder, pressure is 2.0-3.51/cm
2Then 1200 ℃ of sintering 2 hours, the lifting temperature is controlled at 1-1.5 ℃/minute, use slicing machine, the cylinder that sintering is intact is cut into disk, two sides blackening AgPd electrode, divide electrode stamen sheet again into, with behind the stamen sheet welding lead, apply one deck PPS three anti-insulating varnish at stamen sheet and lead-in wire root earlier again, then adopt SWF
12-SB embedding epoxy packages becomes pearl to stop.
The quick resistance electrical parameter of gained pearl body heat R25/50=3950 ± 1%, R25 ℃=83K Ω
Claims (3)
1, a kind of manufacture method of oxidate semi-condcutor thermo-sensitive resistance, it is characterized in that, this manufacture method is: to analyze pure molar percentage % aluminium 3-5, manganese 80-45, the nitrate of nickel 15-52 or acetate are raw material, adopt liquid-phase coprecipitation to prepare the precipitated liquid of material powder, precipitated liquid is the aluminium of concentration 1%, manganese, nickel salt solution, the polyoxyethylene nonylphenol ether that adds weight 1%, under violent stirring, precipitation reagent is evenly added in the precipitated liquid, and precipitation adds that deionized water cleans and solution is carried out sonicated after finishing repeatedly, oven dry, thermal decomposition, levigate, presintering, carry out preforming again, the isostatic cool pressing high temperature sintering is made; In operation must strict control precipitated liquid and the concentration of precipitation reagent carbonic hydroammonium and the ratio of measuring between the two.
According to the manufacture method of the described oxidate semi-condcutor thermo-sensitive resistance of claim 1, it is characterized in that 2, precipitation reagent concentration is the ammonium bicarbonate soln of 1.5-2%, the addition of precipitation reagent is a 2-2.5 times of volume ratio of precipitated liquid.
3, the manufacture method of oxidate semi-condcutor thermo-sensitive resistance according to claim 1 is characterized in that, in thermal decomposition, temperature is 400-500 ℃, time 5-10 hour; In the presintering, temperature is 650-800 ℃; In preforming, material is pre-formed as φ 50mm left and right sides cylinder after, carry out the isostatic cool pressing high temperature sintering, wherein the pressure of isostatic cool pressing is 2.0-3.51/cm
2, 1150-1200 ℃ of high temperature sintering 2 hours, the lifting temperature was controlled at 1-1.5 ℃/minute then; Cylinder disk behind the sintering is cut into slices, and two sides blackening AgPd electrode, scribing are the stamen sheet, and then with behind the stamen sheet employing soldering technology welding lead, apply one deck PPS three at stamen sheet and lead-in wire root earlier and prevent insulating varnish, adopt SWF at last
12-SB type seal ring epoxy resins is dressed up the globule body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97122363A CN1079570C (en) | 1997-12-03 | 1997-12-03 | Oxide semiconductor thermal sensitive resistor and its producing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97122363A CN1079570C (en) | 1997-12-03 | 1997-12-03 | Oxide semiconductor thermal sensitive resistor and its producing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1218964A CN1218964A (en) | 1999-06-09 |
| CN1079570C true CN1079570C (en) | 2002-02-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97122363A Expired - Fee Related CN1079570C (en) | 1997-12-03 | 1997-12-03 | Oxide semiconductor thermal sensitive resistor and its producing method |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107473715B (en) * | 2017-09-27 | 2020-11-20 | 深圳市特普生传感有限公司 | Ternary system NTC thermistor material and manufacturing method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6412501A (en) * | 1987-07-07 | 1989-01-17 | Matsushita Electric Ind Co Ltd | Manufacture of oxide semiconductor for thermistor |
| JPH01290549A (en) * | 1988-05-16 | 1989-11-22 | Ishizuka Denshi Kk | Oxide semiconductor composition for thermistor |
| JPH05135913A (en) * | 1991-11-12 | 1993-06-01 | Matsushita Electric Ind Co Ltd | Manufacture of oxide semiconductor for thermistor |
-
1997
- 1997-12-03 CN CN97122363A patent/CN1079570C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6412501A (en) * | 1987-07-07 | 1989-01-17 | Matsushita Electric Ind Co Ltd | Manufacture of oxide semiconductor for thermistor |
| JPH01290549A (en) * | 1988-05-16 | 1989-11-22 | Ishizuka Denshi Kk | Oxide semiconductor composition for thermistor |
| JPH05135913A (en) * | 1991-11-12 | 1993-06-01 | Matsushita Electric Ind Co Ltd | Manufacture of oxide semiconductor for thermistor |
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| Publication number | Publication date |
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| CN1218964A (en) | 1999-06-09 |
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