CN112820490A - Three-in-one sintering method of strontium titanate annular piezoresistor - Google Patents
Three-in-one sintering method of strontium titanate annular piezoresistor Download PDFInfo
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- CN112820490A CN112820490A CN202110004676.8A CN202110004676A CN112820490A CN 112820490 A CN112820490 A CN 112820490A CN 202110004676 A CN202110004676 A CN 202110004676A CN 112820490 A CN112820490 A CN 112820490A
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000005245 sintering Methods 0.000 title claims abstract description 27
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 title claims abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000007789 gas Substances 0.000 claims abstract description 42
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 33
- 239000001257 hydrogen Substances 0.000 claims abstract description 28
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000001816 cooling Methods 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000004321 preservation Methods 0.000 claims abstract description 24
- 239000003292 glue Substances 0.000 claims abstract description 20
- 238000010304 firing Methods 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- 230000002829 reductive effect Effects 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 5
- 238000012423 maintenance Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000007599 discharging Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 238000005086 pumping Methods 0.000 description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/30—Apparatus or processes specially adapted for manufacturing resistors adapted for baking
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a three-in-one sintering method of a strontium titanate annular piezoresistor, which comprises the following steps: s1: discharging glue, namely, filling the resistor into a box-type furnace, sealing the box-type furnace, introducing air into the box-type furnace chamber, slowly heating the box-type furnace chamber to discharge the glue, and heating the box-type furnace chamber to the temperature A; s2, firing, preserving heat at the temperature A, switching the air of the box furnace into mixed gas of hydrogen and nitrogen during heat preservation, heating to the temperature B for heat preservation or preserving heat at the temperature A, naturally cooling to the temperature C, S3, oxidizing, preserving heat at the temperature C, switching to air during heat preservation, and naturally cooling from the temperature C to the normal temperature after heat preservation. The invention optimizes three required devices into one device, saves the device investment, is completed by only once heating, greatly saves the energy consumption of three times of heating and cooling, saves the manufacturing flow, saves the workshop land and obviously improves the production efficiency.
Description
Technical Field
The invention relates to the technical field of resistor sintering, in particular to a three-in-one sintering method for strontium titanate annular piezoresistor in the processes of binder removal, sintering and oxidation.
Background
The strontium titanate annular piezoresistor for the miniature DC motor is an electronic component with dual functions of voltage sensitivity and high capacitance, and has better performance and larger use amount than a zinc oxide type piezoresistor. Japanese TDK and Taichi occupy high-end markets, domestic factories such as New Laifu and Yili are served by high-middle and low markets, the output of each factory is about 2-10 hundred million per year, and the demand is increased in recent years.
The production of the strontium titanate annular piezoresistor needs to be heated and heated for more than 5 times from raw materials to finished products, the purposes of heating each time are different, the used equipment and working atmosphere are also different, the equipment is mainly an electric furnace, the temperature is not equal to 700-1450 ℃ each time, and the power consumption is large in the mode.
The strontium titanate annular piezoresistor is formed by pressing spray-dried powder by a machine, the powder is bonded, PVA (polyvinyl alcohol) glue needs to be added, therefore, the subsequent sintering needs to be carried out firstly, namely, the PVA glue in the powder is decomposed and discharged by combining with oxygen in the air at a specific temperature, the glue can be discharged at 450 ℃ generally, the temperature is continuously increased to 1000-plus-1200 ℃ for pre-sintering, the resistor is not sticky after the glue is discharged, the mechanical strength is low and fragile, therefore, the temperature needs to be increased to 1000-plus-1200 ℃ for pre-sintering, the resistor has certain mechanical strength and is not fragile, and the subsequent operation is convenient. The glue discharging needs to be carried out in the air atmosphere after the temperature is slowly raised to 1000-1200 ℃ and is kept for a certain time.
In the production process of the resistor, the resistor is fired after glue discharging, the strontium titanate annular piezoresistor is required to have electrical property, firstly, semi-conduction is carried out, the chemical property of the used material is stable, oxygen atoms are difficult to lose, semi-conduction is difficult, and therefore the reduction of hydrogen is required to be utilized and the implementation is carried out under the high-temperature condition. The sintering is a process of utilizing hydrogen to reduce at the high temperature of 1200-1450 ℃. According to the principle, the semi-conduction of the resistor actually loses oxygen, and the oxygen-deprived reductive hydrogen gas is not used in industrial production, and the volume content of the hydrogen is 20-75%. At present, liquid ammonia decomposition gas is used in large-scale production, the volume content of decomposed hydrogen is 75%, the content of nitrogen is 25%, some manufacturers directly use the mixed gas with the proportion content without diluting, and some manufacturers add a certain amount of nitrogen to reduce the hydrogen content. The reduction process needs to be carried out at a temperature of 1200 ℃ or higher in a reducing atmosphere.
After the resistor is subjected to reduction and semiconductor sintering, an oxidation process is required, which is performed in an oxygen-containing atmosphere, generally in the air, at 700-.
In summary, the production process of the strontium titanate annular piezoresistor needs to go through the following steps, the first step is to discharge glue: the second step is sintering at 1000-1200 ℃ in the air: at 1200-: the process is carried out in air at 700-950 ℃, and three continuous processes are carried out in different equipment only because the firing atmosphere of the second step is different. Each step needs to be heated firstly, then is cooled after being kept for a period of time, and the whole process has high energy consumption; the time consumption is 8-24 hours each time, the time is wasted, and different devices are required to be replaced each time, which is very complicated.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides a three-in-one sintering method of a strontium titanate annular piezoresistor, three devices required by sintering of the strontium titanate annular piezoresistor are optimized into one device, the device investment is saved, the traditional production mode needs three heating and cooling processes, so that the energy consumption is large, the time consumption is long, the method is completed only by once heating, the energy consumption for three heating and cooling is greatly saved, the manufacturing process is saved, the plant land is greatly saved, and the production efficiency is obviously improved.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: a three-in-one sintering method of a strontium titanate annular piezoresistor comprises the following steps: s1: removing glue, namely, putting the resistor into a box-type furnace by using a fixture, sealing the box-type furnace, introducing air into the box-type furnace chamber, slowly heating to remove glue, and heating to the temperature A; s2, firing, keeping the temperature at A, switching the air of the box furnace into mixed gas of hydrogen and nitrogen during heat preservation, heating to B for heat preservation or keeping the temperature at A still, naturally cooling to C, S3, oxidizing, keeping the temperature at C, switching the mixed gas of hydrogen and nitrogen in the box furnace into air during heat preservation, and naturally cooling from C to normal temperature after heat preservation.
Preferably, in step S1, air is introduced into the box-type oven cavity, the temperature is raised to D, and after a certain period of heat preservation, the temperature is slowly raised to a temperature a for glue removal, so that the glue removal is more thorough.
Preferably, in step S2, the temperature is maintained at the temperature a, and gas switching is started immediately after the temperature maintenance is started.
Preferably, in step S3, the temperature is maintained at the temperature C, and the gas switching is started immediately after the temperature is decreased to the temperature C.
Preferably, in step S2, the flow rate of the mixed gas is 0.5-2 cubic meters per hour, so as to ensure sufficient hydrogen content in the mixed gas.
Preferably, in step S2, after the heating to the temperature B for heat preservation or the heat preservation still at the temperature a is finished, the flow rate of the hydrogen-nitrogen mixture is adjusted to be 0.01 to 0.1 cubic meter per hour, so as to save the gas amount.
Preferably, when the gas of box-type furnace is switched, the vacuum pump is firstly used for slowly pumping the box-type furnace to negative pressure, nitrogen is filled in, then the negative pressure is pumped, and then the gas to be switched is pumped in, so that the speed of pumping vacuum is not too fast, the gas pumped out too fast is large, heat is brought, the vacuum pump can be burnt out, and the gas can be switched in such a way, so that the gas can be ensured to be switched more thoroughly.
Preferably, when the gas in the box furnace is switched, nitrogen is continuously introduced, the furnace cavity is filled with nitrogen, and then the gas to be switched is introduced.
Preferably, in step S2, the hydrogen gas in the mixed gas is filled to 40% by volume, which ensures sufficient hydrogen reduction.
Preferably, in step S3, when the temperature is naturally decreased from the temperature C to the normal temperature, the flowing air is continuously introduced to accelerate the temperature decrease.
The invention has the following beneficial effects:
the invention optimizes three devices required by the sintering of the strontium titanate annular piezoresistor into one device, saves the device investment, needs three heating and cooling processes in the traditional production mode, has large energy consumption and long time consumption, is completed by heating once, greatly saves the energy consumption of three heating and cooling, saves the manufacturing flow, greatly saves the land for a factory building, and obviously improves the production efficiency.
Detailed Description
The invention will now be further described with reference to specific examples:
example 1:
the first step is as follows: and (3) loading the resistor to be fired into the box-type furnace by using a clamp, closing the door of the box-type furnace, and screwing and sealing. Setting a temperature rise curve, using for 3 hours from normal temperature to 500 ℃, keeping the temperature for 3 hours at 500 ℃ and using for 4 hours from 500 ℃ to 1150 ℃, thus being beneficial to more thorough glue discharging, namely glue discharging in the first step, continuously introducing air for 3 cubic meters per hour through an air hole arranged at the bottom of the furnace, wherein the air flows, enters the air from the bottom of the furnace body, and exits from the top of the furnace body, thus being glue discharging in the first step.
The second step is that: keeping the temperature at 1150 ℃ for one hour, wherein the one hour is used for atmosphere conversion time, slowly pumping the box type furnace by a vacuum pump until the air pressure in the furnace is-80 kPa, under the negative pressure, oxygen in the box-type furnace is remained a little, the vacuumizing speed cannot be too fast, the gas pumped out too fast is large, the heat is much, the vacuumizing pump is burnt out, nitrogen is introduced to the normal pressure, the gas is pumped into the furnace again until the gas pressure is minus 80 kilopascals, the nitrogen is introduced again until the normal pressure, the oxygen content in the furnace is little, the nitrogen-hydrogen mixed gas containing 30% of hydrogen by volume is introduced, the gas flow is 0.5 cubic meter per hour, heating is continued, the time is 2 hours from 1150 ℃ to 1400 ℃, the temperature is preserved for 5 hours at 1400 ℃, naturally cooling to 900 ℃, introducing hydrogen in the process for reduction, sintering in the second step, after the heat preservation at 1400 ℃, the flow of the hydrogen-nitrogen mixture can be regulated to be as small as 0.01 cubic meter per hour so as to save the consumption of the hydrogen.
The third step: keeping the temperature at 900 ℃ for 4 hours, when the temperature is just reduced to the temperature, slowly pumping the box-type furnace by a vacuum pump again until the air pressure in the furnace reaches-80 kilopascals, introducing nitrogen to the normal pressure when little hydrogen remains in the box-type furnace under the negative pressure, pumping the box-type furnace again until the air pressure in the furnace reaches-80 kilopascals, introducing nitrogen to the normal pressure, introducing little hydrogen into the furnace at the moment, introducing air for 1 cubic meter per hour, naturally cooling to the normal temperature after the temperature preservation at 900 ℃, which is the oxidation process of the third step, stopping introducing air in the final natural cooling process, and continuously introducing air to facilitate cooling and quickening the cooling.
Example 2:
the first step is as follows: and (3) loading the resistor to be fired into the box-type furnace by using a clamp, closing the door of the box-type furnace, and screwing and sealing. Setting a heating curve, using for 7 hours at the normal temperature of-1200 ℃, continuously introducing air for 2 cubic meters per hour through an air hole arranged at the bottom of the furnace in the heating process, wherein the air flows, enters air from the bottom of the furnace body, and exits air from the top of the furnace body, which is the glue discharging in the first step.
The second step is that: keeping the temperature at 1200 ℃ for one hour, wherein the hour is used for atmosphere conversion time, introducing nitrogen through a gas hole arranged at the bottom of the furnace, the flow rate of the nitrogen is 4 cubic meters per hour, after introducing the nitrogen for 1 hour, the oxygen content in the furnace is less at the moment, introducing nitrogen-hydrogen mixed gas containing 40% of hydrogen by volume, the flow rate of the nitrogen-hydrogen mixed gas is 1.5 cubic meters per hour, continuing to heat the mixture for 1 hour from 1200-1350 ℃, keeping the temperature at 1350 ℃ for 5 hours, naturally cooling the mixture to 800 ℃, introducing the firing of the second step of hydrogen reduction, and after keeping the temperature at 1350 ℃, reducing the flow rate of the hydrogen-nitrogen mixed gas to 0.03 cubic meters per hour to save the gas.
The third step: and (2) preserving the temperature at 800 ℃ for 4 hours, wherein when the temperature in the furnace is just reduced to the temperature, nitrogen is introduced through air holes arranged at the bottom of the furnace, the flow rate is 4 cubic meters per hour, after the nitrogen is introduced for 1 hour, the content of hydrogen in the furnace is very low, air is introduced for 1 cubic meter per hour, and after the temperature preservation at 800 ℃, the temperature is naturally reduced to the normal temperature, which is the oxidation process in the third step. In the final natural cooling process, the air can be stopped from being introduced, and the air can also be continuously introduced to facilitate cooling and accelerate cooling.
Example 3:
the first step is as follows: and (3) loading the resistor to be fired into the box-type furnace by using a clamp, closing the door of the box-type furnace, and screwing and sealing. Setting a heating curve, using for 8 hours from normal temperature to 1360 ℃, continuously introducing air for 1.5 cubic meters per hour through an air hole arranged at the bottom of the furnace in the heating process, wherein the air flows, enters the furnace body from the bottom of the furnace body, and exits from the top of the furnace body, which is the glue discharging of the first step.
The second step is that: keeping the temperature at 1360 ℃ for 6 hours, using the temperature for atmosphere conversion time at the beginning of one hour, slowly pumping the box type furnace by a vacuum pump until the air pressure in the furnace is-80 kPa, under the negative pressure, the oxygen in the box-type furnace is remained a little, the vacuumizing speed cannot be too fast, the gas pumped out too fast is large, the heat is more, the vacuumizing pump is burnt out, the nitrogen is introduced to the normal pressure, then pumping the box-type furnace again until the air pressure in the furnace is minus 80 kPa, introducing nitrogen again to the normal pressure, introducing nitrogen-hydrogen mixed gas containing 60 percent of hydrogen by volume ratio at the moment that the oxygen content in the furnace is little, the flow rate is 2 cubic meters per hour, the heat preservation is continuously carried out at 1360 ℃, after the heat preservation is finished, the temperature is naturally reduced to 900 ℃, the second step of firing of hydrogen reduction is introduced in the process, after the heat preservation at 1360 ℃ is finished, the flow rate of the hydrogen-nitrogen mixed gas can be adjusted to be as small as 0.1 cubic meter per hour so as to save the hydrogen consumption.
The third step: keeping the temperature at 900 ℃ for 4 hours, when the temperature is just reduced to the temperature, slowly pumping the box-type furnace by a vacuum pump again until the air pressure in the furnace reaches-80 kilopascals, introducing nitrogen to the normal pressure, pumping the gas again until the air pressure in the furnace reaches-80 kilopascals, introducing nitrogen to the normal pressure under the negative pressure till little hydrogen remains in the box-type furnace, introducing air for 2 cubic meters per hour at the moment, and naturally cooling to the normal temperature after the temperature of 900 ℃ is maintained, which is the oxidation process in the third step. In the final natural cooling process, the air can be stopped from being introduced, and the air can also be continuously introduced to facilitate cooling and accelerate cooling.
The above-mentioned embodiments are merely preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, so that variations based on the shape and principle of the present invention should be covered within the scope of the present invention.
Claims (10)
1. A three-in-one sintering method of a strontium titanate annular piezoresistor is characterized by comprising the following steps: s1: removing glue, namely, putting the resistor into a box-type furnace by using a fixture, sealing the box-type furnace, introducing air into the box-type furnace chamber, slowly heating to remove glue, and heating to the temperature A; s2, firing, keeping the temperature at A, switching the air of the box furnace into mixed gas of hydrogen and nitrogen during heat preservation, heating to B for heat preservation or keeping the temperature at A still, naturally cooling to C, S3, oxidizing, keeping the temperature at C, switching the mixed gas of hydrogen and nitrogen in the box furnace into air during heat preservation, and naturally cooling from C to normal temperature after heat preservation.
2. The three-in-one sintering method of the strontium titanate annular piezoresistor according to claim 1, characterized in that: in step S1, air is introduced into the box-type furnace chamber, the temperature is raised to D, and after a certain period of heat preservation, the temperature is slowly raised to a temperature a for glue removal.
3. The three-in-one sintering method of the strontium titanate annular piezoresistor according to claim 1, characterized in that: in step S2, the temperature is maintained at the temperature a, and gas switching is started immediately after the temperature maintenance is started.
4. The three-in-one sintering method of the strontium titanate annular piezoresistor according to claim 1, characterized in that: in step S3, the temperature is maintained at the temperature C, and the gas switching is started immediately after the temperature is lowered to the temperature C.
5. The three-in-one sintering method of the strontium titanate annular piezoresistor according to claim 1, characterized in that: in step S2, the flow rate of the hydrogen-nitrogen mixed gas is 0.5 to 2 cubic meters per hour.
6. The three-in-one sintering method of the strontium titanate annular piezoresistor according to claim 5, characterized in that: in the step S2, after the temperature is heated to the temperature B for heat preservation or the temperature A is still used for heat preservation, the flow of the hydrogen-nitrogen mixture is adjusted to be 0.01-0.1 cubic meter per hour.
7. The three-in-one sintering method of the strontium titanate annular piezoresistor according to claim 1, characterized in that: when the gas of the box-type furnace is switched, the box-type furnace is slowly pumped to negative pressure by a vacuum pump, nitrogen is filled to normal pressure, then the box-type furnace is pumped to negative pressure, the box-type furnace is filled with nitrogen again to normal pressure, and the gas to be switched is switched.
8. The three-in-one sintering method of the strontium titanate annular piezoresistor according to claim 1, characterized in that: when the gas of the box-type furnace is switched, firstly, nitrogen is continuously introduced, the furnace cavity is filled with the nitrogen, and then, the gas to be switched is introduced.
9. The three-in-one sintering method of the strontium titanate annular piezoresistor as claimed in claims 1-8, wherein: in step S2, the hydrogen gas in the filled mixed gas accounts for 30-60% by volume.
10. The three-in-one sintering method of the strontium titanate annular piezoresistor according to any one of claims 1-8, characterized in that: and in the step S3, when the temperature is naturally reduced from the temperature C to the normal temperature, continuously introducing air to accelerate the temperature reduction speed.
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CN1297233A (en) * | 1999-11-18 | 2001-05-30 | 原培新 | Method for producing MFC-series high-dielectric voltage-sensitive resistor/capacitor compound element |
CN1800091A (en) * | 2005-12-31 | 2006-07-12 | 昆明理工大学 | Method for producing nanometer doping agent modified SrTiO3 pressure sensitive ceramic material ,resistance and the resistance produced therefrom |
CN1828846A (en) * | 2006-01-16 | 2006-09-06 | 山东师范大学 | Oxidation and gallium diffusion one-stepped operation process for manufacturing semiconductor device |
CN103319172A (en) * | 2013-06-14 | 2013-09-25 | 广东风华高新科技股份有限公司 | Annular piezoresistor ceramic and preparation method thereof, and annular piezoresistor and preparation method thereof |
CN108461293A (en) * | 2018-04-09 | 2018-08-28 | 广东风华高新科技股份有限公司 | A kind of manufacturing method of ceramic capacitor |
CN112097523A (en) * | 2020-09-21 | 2020-12-18 | 盐城工学院 | Atmosphere box type sintering furnace for production of mobile phone back plate |
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2021
- 2021-01-04 CN CN202110004676.8A patent/CN112820490A/en active Pending
Patent Citations (6)
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CN1297233A (en) * | 1999-11-18 | 2001-05-30 | 原培新 | Method for producing MFC-series high-dielectric voltage-sensitive resistor/capacitor compound element |
CN1800091A (en) * | 2005-12-31 | 2006-07-12 | 昆明理工大学 | Method for producing nanometer doping agent modified SrTiO3 pressure sensitive ceramic material ,resistance and the resistance produced therefrom |
CN1828846A (en) * | 2006-01-16 | 2006-09-06 | 山东师范大学 | Oxidation and gallium diffusion one-stepped operation process for manufacturing semiconductor device |
CN103319172A (en) * | 2013-06-14 | 2013-09-25 | 广东风华高新科技股份有限公司 | Annular piezoresistor ceramic and preparation method thereof, and annular piezoresistor and preparation method thereof |
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