CN100378873C - Zinc coped negative temperature coefficient single crystal silicon thermo sensitive resistor - Google Patents
Zinc coped negative temperature coefficient single crystal silicon thermo sensitive resistor Download PDFInfo
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- CN100378873C CN100378873C CNB2004100920274A CN200410092027A CN100378873C CN 100378873 C CN100378873 C CN 100378873C CN B2004100920274 A CNB2004100920274 A CN B2004100920274A CN 200410092027 A CN200410092027 A CN 200410092027A CN 100378873 C CN100378873 C CN 100378873C
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Abstract
The present invention relates to a negative temperature coefficient monocrystal silicon thermistor doped with zinc, which uses a vacuum gas phase diffusion method. Zinc atoms are used as dopants and are doped in n-shaped monocrystal silicon. A bead-shaped thermistor with high B value is prepared by the impurity compensation property of zinc in the n-shaped monocrystal silicon. The thermistor is suitable for an element of a thermometer (such as a clinical thermometer) of which the thermistor must have high B value. The thermal sensitive element used by a paster technology of the upper surface of an integrated circuit board requires to use a chip type element with high B value. In equipment, such as motors, etc., a strong surge current needs inhibiting during machine starting for protecting the equipment. Various kinds of charging equipment needs using the thermistor with high B value so as to inhibit the surge current for prolonging the service life of a battery.
Description
Technical field
The present invention relates to a kind of negative temperature coefficient monocrystalline silicon thermistor of zinc doping.
Background technology
Functional material and sensor technology are one of three big industries of China's information technology.Because negative temperature coefficient heat-sensitive resistance material has than higher sensitivity (B value) temperature, therefore the thermistor element made from this material is most important in the sensor technology always, application surface is the widest, and a class transducer with fastest developing speed is by being paid attention to countries in the world.
Thermistor element has formed an independently industry at present, and the annual consumption in the whole world reaches 2,000,000,000, hundred million of the about 3-4 of domestic annual consumption, and annual speed increment with 15-20%.Expect 2010, China will become in the world the big country that produces, uses and sell thermistor, and domestic consumption will reach more than 1,000,000,000.And present domestic annual output only is about 1.5 hundred million, and the 60-70% of domestic market is occupied by the product of countries such as Japan, Korea S, the U.S..
Along with information technology and electrified popularizing and development, the consumption of thermistor and kind will increase considerably, and particularly some high accuracy, high B value/low resistance thermistor element and transducer will become the undersupplied product of the sector.People are for the class that improves element with satisfy the demand of market to high B value/low resistance special components for many years, have adopted that doped with rare-earth elements, element adopt technology such as multilayer and string structure in making in oxide material, but do not obtain the result that is satisfied with so far.And silicon single crystal thermal sensitive resistor is having more advantage and competitiveness than oxide thermosensitive resistor aspect sensitivity, production efficiency and the manufacturing cost, and the silicon single crystal thermal sensitive resistor of particularly high B value/low resistance has very strong advantage.About preparing the silicon single crystal thermo-sensitive material,, still fail so far to develop and industrialization though there are some researchs in the past with the transition metal ions compensation technique.
At present, the temperature-sensitive functional material that uses of each manufacturer all is that oxide with transition metal is (as Co both at home and abroad
3O
4, Mn
2O
3, Fe
2O
3, NiO, CuO etc.) mixture be parent material, or directly use the powder of metal oxide, or produce metal oxide by chemical coprecipitation, sol-gel process by slaine, prepare thermo-sensitive material through briquetting sintering, curtain coating or calendering technology.Its subject matter is that the composition and the phase structure of this composite material is inhomogeneous, and porosity height directly influences consistency, repeatability and the reliability of thermistor element.And according to the intrinsic rule of polycrystalline oxide semiconductor, when material coefficient B value (Δ E/k) was high, resistivity was inevitable also high, therefore is difficult to realize high B value/low resistance characteristic with this material.
In recent years, great effort has been done for solving consistency, repeatability and integrity problem by research institution and manufacturer on material preparation and component manufacturing technology both at home and abroad, though obtain certain effect, does not tackle the problem at its root yet.Be mixed with the compensation Si semiconductor of deep-level impurity, its resistivity has the different sensitiveness of degree to temperature, its sensitivity coefficient B value is relevant with the level of energy and the doping content of deep-level impurity, so just might obtain high B value material by selecting suitable impurity and concentration.The resistivity of the compensation silicon thermo-sensitive material of same material coefficient B value is more much smaller than the oxide material, so just can produce the monocrystalline silicon thermistor element of high B value low resistance.
Up to now, directly related with mix zinc compensation technique exploitation thermistor material and element with silicon single crystal research is not reported.And the research of indirect correlation has: doping deep-level impurity gold improves the research of devices switch speed and frequency characteristic in semi-conducting materials such as Si, Ge, and doping gold or manganese form the report of thermo-sensitive material in silicon.Nineteen eighty-three, Toshiba Corp developed the silicon doped gold thermistor, obtained B=4300K, R=15k Ω; 85102901.9 1 kinds of silicon doped gold thermistors of Chinese patent and manufacture method; Chinese patent 87103486.3 gold dopings, mix the platinum monocrystalline silicon thermistor; The negative temperature coefficient monocrystalline silicon thermistor that CN200310116749.4 manganese mixes.But these researchs all do not relate to the research of doping deep-level impurity zinc, do not relate to the exploitation that the doping that utilizes low melting point, deep-level impurity prepares high B value/low resistance thermo-sensitive material yet.
Summary of the invention
The object of the invention is, the negative temperature coefficient monocrystalline silicon thermistor of a kind of zinc doping of development, this thermistor adopt vacuum gas phase diffusion method, and zinc atom as dopant, is mixed in the n type monocrystalline silicon; Utilize the impurity compensation character of zinc in n type monocrystalline silicon, prepare the high B value of pearl thermistor.This resistor is applicable to thermometer (as clinical thermometer), and employed thermistor must be the element of high B value; On surface-mounted integrated circuit, the employed temperature-sensitive element of surface patch technology requires to adopt high B value slice formula element; In equipment such as motor, this resistor stronger surge current when being used to suppress machine startup is protected equipment; In all kinds of charging devices, use the thermistor of the high B value of this resistor can suppress surge current, extend the life of a cell.
The negative temperature coefficient monocrystalline silicon thermistor of a kind of zinc doping of the present invention, this thermistor adopt vacuum gas phase diffusion method, and zinc atom as dopant, is mixed in the n type monocrystalline silicon; Utilize the impurity compensation character of zinc in n type monocrystalline silicon, prepare the high B value of pearl thermistor, electrical parameter is 1.5K Ω-24K Ω, material coefficient B value 3000-6350K.
A kind of preparation method of negative temperature coefficient monocrystalline silicon thermistor of zinc doping follows these steps to carry out:
A, employing resistivity are the n type monocrystalline silicon piece of 0.1-30 Ω cm, with 80 order diamond dust the two sides are polished, polish;
B, silicon chip is put into deionized water ultrasonic waves for cleaning shakeout, boil with chloroazotic acid then, use washed with de-ionized water again;
C, the silicon chip of handling well is put into the quartz ampoule of end sealing, add diffuse source metallic zinc 6-20 milligram again, quartz ampoule is evacuated to 1.33 * 10
-2More than the Pa, seal;
The flat-temperature zone that d, the quartz ampoule that silicon chip and diffuse source will be housed are put into high temperature dispersing furnace spreads, and the temperature drift of diffusion furnace flat-temperature zone is no more than ± and 1 ℃, diffusion temperature is 1100 ℃-1300 ℃, be 5-10 hour diffusion time;
E, diffusion are taken out quartz ampoule after finishing immediately, break quartz ampoule behind the chilling and take out silicon chip;
F, adopt the technology of step a and b, carry out HF immersion, polishing, shakeout, the processing of deoiling spreading good silicon chip;
G, plating Ni electrode are in a vacuum with 400-600 ℃ of annealing;
H, be divided into small pieces, use epoxy encapsulation with scribing machine;
I, the relation in thermostatic oil bath between testing element resistance and the temperature are carried out 0.01 ℃ of constant temperature precision under the zero energy condition;
J, in baking oven, carry out under 100 ℃ of temperature 100 hours aging.
Silicon temperature-sensitive functional material is based on the silicon single crystal semiconductor, and doping special metal atom forms the deep energy level trapping centre, makes the material production sensitive characteristic.This material does not exist crystal grain, crystal boundary, pore and distributes mutually, and the uniformity of material, consistency and repeatability are better than oxide ceramic material.Through concentration and the distribution thereof of strict controlled doping atom in silicon, be easy to realize the high B value element that is difficult to realize with the oxide ceramics thermo-sensitive material and consistency, repeatability, the stability of raising thermo-sensitive material and element.
Major technique of the present invention is that the low boiling metallic zinc is mixed in the n type silicon single crystal, forms deep acceptor impurity trapping centre, captures the portions of electronics in the conduction band.When material temperature raise, some trapped electron thermal excitations changed resistivity of material to conduction band, thereby present sensitive characteristic.Because the boiling point that zinc is depressed at standard atmosphere has only 907 ℃, be very suitable for mixing with high temperature gas phase method of diffusion, and the level of energy of zinc impurity in the silicon band gap also is suitable for obtaining the thermo-sensitive material of high B value very much.
The negative temperature coefficient monocrystalline silicon thermistor of a kind of zinc doping of the present invention has following characteristics:
1, selected new dopant: select boiling point zinc relatively low, that in silicon, can form deep energy level as dopant, mix in the n type monocrystalline silicon.Because the boiling point of zinc only is 907 ℃, created advantage in High temperature diffusion, improving the consistency and the uniformity of mixing.As long as adopt suitable diffusion temperature and time, just can be made into all reasonable thermo-sensitive material of consistency, repeatability.
2, adopted vacuum stopped pipe technology: silicon single crystal is mixed zinc and is adopted vacuum stopped pipe diffusion technology, at first the silicon chip that will handle and high-purity zinc powder are put into quartz ampoule, and pumping high vacuum also seals, and form stopped pipe, heat evenly spreads zinc then, promptly makes thermistor material.Its technology is simple, and is easy to operate.
3, change material parameter by changing the diffuse source input amount: for oxide thermosensitive resistor, the B value is changed, need by changing prescription, warming and cooling rate, conditions such as thermostat temperature and time realize.And for the monocrystalline silicon thermistor of mixing zinc, by changing the input amount of diffuse source zinc, thermostat temperature and constant temperature time can make resistance and B value change.
4, prepare high B value thermistor composition: utilize the impurity compensation character of zinc in n type monocrystalline silicon, prepare high B value material.
Embodiment
Embodiment 1
A, employing resistivity are the n type monocrystalline silicon piece of 0.1 Ω cm, with 80 order diamond dust the two sides are polished, polish;
B, silicon chip is put into deionized water ultrasonic waves for cleaning shakeout, boil with chloroazotic acid then, use washed with de-ionized water again;
C, the silicon chip of handling well is put into the quartz ampoule of end sealing, add 16 milligrams of diffuse source metallic zinc again, quartz ampoule is evacuated to 1.33 * 10
-2More than the Pa, seal;
The flat-temperature zone that d, the quartz ampoule that silicon chip and diffuse source will be housed are put into high temperature dispersing furnace spreads, and the temperature drift of diffusion furnace flat-temperature zone is no more than ± and 1 ℃, according to the different performance requirement, diffusion temperature is chosen in 1250 ℃, is chosen in 10 hours diffusion time;
E, diffusion are taken out quartz ampoule after finishing immediately, break quartz ampoule behind the chilling and take out silicon chip;
F, adopt the technology of step a and b, carry out HF immersion, polishing, shakeout, the processing of deoiling spreading good silicon chip;
G, plating Ni electrode are in a vacuum with 600 ℃ of annealing;
H, be divided into small pieces, use epoxy encapsulation with scribing machine;
I, the relation in thermostatic oil bath between testing element resistance and the temperature are carried out 0.01 ℃ of constant temperature precision under the zero energy condition;
J, in baking oven, carry out under 100 ℃ of temperature 100 hours aging.
Electrical parameter is 24K Ω, material coefficient B value 6350K.
Embodiment 2
A, employing resistivity are the n type monocrystalline silicon piece of 3 Ω cm, with 80 order diamond dust the two sides are polished, polish;
B, silicon chip is put into deionized water ultrasonic waves for cleaning shakeout, boil with chloroazotic acid then, use washed with de-ionized water again;
C, the silicon chip of handling well is put into the quartz ampoule of end sealing, add 10 milligrams of diffuse source metallic zinc again, quartz ampoule is evacuated to 1.33 * 10
-2More than the Pa, seal;
The flat-temperature zone that d, the quartz ampoule that silicon chip and diffuse source will be housed are put into high temperature dispersing furnace spreads, and the temperature drift of diffusion furnace flat-temperature zone is no more than ± and 1 ℃, according to the different performance requirement, diffusion temperature is chosen in 1100 ℃, is chosen in 5 hours diffusion time;
E, diffusion are taken out quartz ampoule after finishing immediately, break quartz ampoule behind the chilling and take out silicon chip;
F, adopt the technology of step a and b, carry out HF immersion, polishing, shakeout, the processing of deoiling spreading good silicon chip;
G, plating Ni electrode are in a vacuum with 500 ℃ of annealing;
H, be divided into small pieces, use epoxy encapsulation with scribing machine;
I, the relation in thermostatic oil bath between testing element resistance and the temperature are carried out 0.01 ℃ of constant temperature precision under the zero energy condition;
J, in baking oven, carry out under 100 ℃ of temperature 100 hours aging.
Electrical parameter is 10K Ω, material coefficient B value 6200K.
Embodiment 3
A, employing resistivity are the n type monocrystalline silicon piece of 30 Ω cm, with 80 order diamond dust the two sides are polished, polish;
B, silicon chip is put into deionized water ultrasonic waves for cleaning shakeout, boil with chloroazotic acid then, use washed with de-ionized water again;
C, the silicon chip of handling well is put into the quartz ampoule of end sealing, add 20 milligrams of diffuse source metallic zinc again, quartz ampoule is evacuated to 1.33 * 10
-2More than the Pa, seal;
The flat-temperature zone that d, the quartz ampoule that silicon chip and diffuse source will be housed are put into high temperature dispersing furnace spreads, and the temperature drift of diffusion furnace flat-temperature zone is no more than ± and 1 ℃, according to the different performance requirement, diffusion temperature is chosen in 1200 ℃, is chosen in 10 hours diffusion time;
E, diffusion are taken out quartz ampoule after finishing immediately, break quartz ampoule behind the chilling and take out silicon chip;
F, adopt the technology of step a and b, carry out HF immersion, polishing, shakeout, the processing of deoiling spreading good silicon chip;
G, plating Ni electrode are in a vacuum with 400 ℃ of annealing;
H, be divided into small pieces, use epoxy encapsulation with scribing machine;
I, the relation in thermostatic oil bath between testing element resistance and the temperature are carried out 0.01 ℃ of constant temperature precision under the zero energy condition;
J, in baking oven, carry out under 100 ℃ of temperature 100 hours aging.
Electrical parameter is 1.5K Ω, material coefficient B value 3000K.
Embodiment 4
A, employing resistivity are the n type monocrystalline silicon piece of 15 Ω cm, with 80 order diamond dust the two sides are polished, polish;
B, silicon chip is put into deionized water ultrasonic waves for cleaning shakeout, boil with chloroazotic acid then, use washed with de-ionized water again;
C, the silicon chip of handling well is put into the quartz ampoule of end sealing, add 6 milligrams of diffuse source metallic zinc again, quartz ampoule is evacuated to 1.33 * 10
-2More than the Pa, seal;
The flat-temperature zone that d, the quartz ampoule that silicon chip and diffuse source will be housed are put into high temperature dispersing furnace spreads, and the temperature drift of diffusion furnace flat-temperature zone is no more than ± and 1 ℃, according to the different performance requirement, diffusion temperature is chosen in 1250 ℃, is chosen in 8 hours diffusion time;
E, diffusion are taken out quartz ampoule after finishing immediately, break quartz ampoule behind the chilling and take out silicon chip;
F, adopt the technology of step a and b, carry out HF immersion, polishing, shakeout, the processing of deoiling spreading good silicon chip;
G, plating Ni electrode are in a vacuum with 450 ℃ of annealing;
H, be divided into small pieces, use epoxy encapsulation with scribing machine;
I, the relation in thermostatic oil bath between testing element resistance and the temperature are carried out 0.01 ℃ of constant temperature precision under the zero energy condition;
J, in baking oven, carry out under 100 ℃ of temperature 100 hours aging.
Electrical parameter is 5K Ω, material coefficient B value 4500K.
Claims (2)
1. the negative temperature coefficient monocrystalline silicon thermistor of a zinc doping is characterized in that this thermistor adopts vacuum gas phase diffusion method, as dopant, mixes zinc atom in the n type monocrystalline silicon; Utilize the impurity compensation character of zinc in n type monocrystalline silicon, prepare the high B value of pearl thermistor, electrical parameter is 1.5K Ω-24K Ω, material coefficient B value 30006350K.
2. the preparation method of the negative temperature coefficient monocrystalline silicon thermistor of a kind of zinc doping according to claim 1 is characterized in that following these steps to carrying out:
A, employing initial electrical resistivity are the n type monocrystalline silicon piece of 0.1-30 Ω cm, with 80 order diamond dust the two sides are polished, polish;
B, silicon chip is put into deionized water ultrasonic waves for cleaning shakeout, boil with chloroazotic acid then, use washed with de-ionized water again;
C, the silicon chip of handling well is put into the quartz ampoule of end sealing, add diffuse source metallic zinc 6-20 milligram again, quartz ampoule is evacuated to 1.33 * 10
-2More than the Pa, seal;
The flat-temperature zone that d, the quartz ampoule that silicon chip and diffuse source will be housed are put into high temperature dispersing furnace spreads, and the temperature drift of diffusion furnace flat-temperature zone is no more than ± and 1 ℃, diffusion temperature is 1100 ℃-1300 ℃, be 5-10 hour diffusion time;
E, diffusion are taken out quartz ampoule after finishing immediately, break quartz ampoule behind the chilling and take out silicon chip;
F, carry out HF and soak, adopt the technology of step a and b again, the two sides is polished, polishes, put into deionized water ultrasonic waves for cleaning shakeout, boil with chloroazotic acid then, use the deionized water clean again with diamond dust to spreading good silicon chip;
G, plating Ni electrode are in a vacuum with 400-600 ℃ of annealing;
H, be divided into small pieces, use epoxy encapsulation with scribing machine;
I, the relation in thermostatic oil bath between testing element resistance and the temperature are carried out 0.01 ℃ of constant temperature precision under the zero energy condition;
J, in baking oven, carry out under 100 ℃ of temperature 100 hours aging.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100920274A CN100378873C (en) | 2004-11-05 | 2004-11-05 | Zinc coped negative temperature coefficient single crystal silicon thermo sensitive resistor |
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|---|---|---|---|
| CNB2004100920274A CN100378873C (en) | 2004-11-05 | 2004-11-05 | Zinc coped negative temperature coefficient single crystal silicon thermo sensitive resistor |
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| CN100378873C true CN100378873C (en) | 2008-04-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495942A (en) * | 2014-12-31 | 2015-04-08 | 郑州大学 | Negative thermal expansion material NdMnO3 and preparation method thereof |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101136271B (en) * | 2007-10-24 | 2010-06-09 | 中国科学院新疆理化技术研究所 | Transient metal multiple adulterate negative temperature coefficient monocrystalline silicon thermistor |
| CN101786861B (en) * | 2009-12-28 | 2012-09-05 | 中国科学院新疆理化技术研究所 | Negative temperature coefficient thermosensitive resistor with high resistance and low B value |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87103486A (en) * | 1987-05-07 | 1988-01-13 | 中国科学院新疆物理研究所 | Gold doping, mix platinum single crystal silicon interchangeable thermistor and preparation method thereof |
| JP2002100504A (en) * | 2000-09-22 | 2002-04-05 | Mitsubishi Materials Corp | Electronic component comprising composite-type semiconductor ceramic material |
| US20020074657A1 (en) * | 2000-10-11 | 2002-06-20 | Murata Manufacturing Co., Ltd. | Semiconductor ceramic having a negative temperature coefficient of resistance and negative temperature coefficient thermistor |
-
2004
- 2004-11-05 CN CNB2004100920274A patent/CN100378873C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87103486A (en) * | 1987-05-07 | 1988-01-13 | 中国科学院新疆物理研究所 | Gold doping, mix platinum single crystal silicon interchangeable thermistor and preparation method thereof |
| JP2002100504A (en) * | 2000-09-22 | 2002-04-05 | Mitsubishi Materials Corp | Electronic component comprising composite-type semiconductor ceramic material |
| US20020074657A1 (en) * | 2000-10-11 | 2002-06-20 | Murata Manufacturing Co., Ltd. | Semiconductor ceramic having a negative temperature coefficient of resistance and negative temperature coefficient thermistor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495942A (en) * | 2014-12-31 | 2015-04-08 | 郑州大学 | Negative thermal expansion material NdMnO3 and preparation method thereof |
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