CN106747405A - A kind of high stability zinc oxide varistor preparation method - Google Patents
A kind of high stability zinc oxide varistor preparation method Download PDFInfo
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- CN106747405A CN106747405A CN201710070179.1A CN201710070179A CN106747405A CN 106747405 A CN106747405 A CN 106747405A CN 201710070179 A CN201710070179 A CN 201710070179A CN 106747405 A CN106747405 A CN 106747405A
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- H01C7/00—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
- H01C7/10—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 voltage responsive, i.e. varistors
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Abstract
The invention belongs to production process of electronic elements technical field.It is related to a kind of universal zinc oxide varistor high stability zinc oxide varistor preparation method.The method includes the step of dispensing, ball milling, granulation, shaping, sintering, electrode processed and welding encapsulating, and in batching step, below 0.4 micron, other doping material are using the raw material that d50 is below 1.0 microns and purity is more than 99.7% for the d50 of the zinc oxide of use.The present invention improves raw material, is formulated adjustment, increases Ball-milling Time, increase product safety surplus, greatly improves product stability;After direct current ceiling temperature endurancing 1000 hours before by improving, generally more than 10.0 microamperes, after direct current ceiling temperature endurancing to after improving 1000 hours, leakage current is generally below 3.0 microamperes for leakage current.
Description
Technical field
The invention belongs to production process of electronic elements technical field.It is related to a kind of universal zinc oxide varistor high steady
Qualitative zinc oxide varistor preparation method.
Background technology
By the development of 30 or 40 years, piezoresistor has been a kind of product of comparative maturity, is widely used in family expenses
The field such as electrical equipment, electric instrument and equipment, communication, thunder resisting equipment, LED, by long-term use, undergo abnormal overvoltage,
Several failure of ten thousand/several or hundreds of thousands point is had after high environment temperature etc., and is wherein caused because stability is bad
Product failure is major part.It is also what is be impermissible for for a certain equipment although probability very little.Piezoresistor failure
Phenomenon be piezo-resistance short circuit, blast, flare scurry out, cause other components even whole equipment it is on fire or burning.How
Significantly reduce failure ratio, be have problem to be solved.
The content of the invention
In order to solve the problems, such as prior art, it is not change original process equipment that the present invention needs the problem for solving
Under conditions of, there is provided a kind of method that can improve piezoresistor stability.By improving product stability, reduce product bad
Change, so as to significantly reduce failure ratio.
Conventional zinc oxide varistor preparation method includes dispensing, ball milling, granulation, shaping, sintering, electrode processed and weldering
The step of connecing encapsulating, in order to solve the above technical problems, the present invention is achieved through the following technical solutions:A kind of high stability
Zinc oxide varistor preparation method, including the step of dispensing, ball milling, granulation, shaping, sintering, electrode processed and welding encapsulating,
It is characterized in that:In batching step, below 0.4 micron, bismuth oxide, three are expected in other doping to the d50 of the zinc oxide of use
Two antimony, cobaltosic oxide, chrome green, nickel sesquioxide, manganese oxide are aoxidized using d50 is below 1.0 microns and purity exists
More than 99.7% raw material;The Ball-milling Time of ball milling step is 6 hours.
In the inventive method batching step, the content of silver-colored glass powder is the 0.1% of zinc oxide in formula;Chromic oxide content
It is the 0.24% of zinc oxide.
Dispersant is made using deflocculant A-15 in the inventive method ball milling step.
In the inventive method sintering step by the way of sintering temperature is adjusted again after prerun burning, during control pressure sensitive voltage takes
Center value around and above (- 2% to+10%.).It is the chargeability for reducing product with realization, increases safe clearance, so as to improve product
The service life of product.
The present invention improves pulping process (including dispensing, ball milling) by adjusting Product Process formula.1st, doping material is (except main
Other materials beyond material oxidation zinc) use ultra-fine, high pure raw material, zinc oxide obtained in indirect method obtain d50 0.4 micron with
Under, this patent be exactly by d50 generally more than 2.0 microns and bismuth oxide, antimony oxide, four of the purity 98% or so
Co 3 O, chrome green, nickel sesquioxide, manganese oxide etc. be changed to d50 below 1.0 microns and purity 99.7% with
On.2nd, increase slurrying Ball-milling Time, high speed Ball-milling Time was increased to 6 hours by original 2 hours, mix slurry more equal
Even, more preferably, be more convenient for granulation and powder are uniform for slurry fluidity.3rd, increasing in being formulated can improve the material of product stability:Silver
Glass powder, chromium oxide, silver-colored glass powder in being typically formulated, chromium oxide (i.e. chrome green) content improves 50%, improves rear oxidation chromium
Content reach the 0.24% of zinc oxide.Chromium oxide can enter the zinc of antimony oxide and zinc oxide reaction generation in crystal boundary
In antimony spinelle, and this zinc antimony spinelle can be made more stable, in the case where long term high temperature is powered, be difficult structural change, from
And make crystal boundary stabilization, properties of product stabilization.4th, conventional method typically uses Home-Made Disperse agent, and we use by test of many times makes
Make dispersant with the deflocculant A-15 of Britain's technique productions, polarity sequence is more preferably, (general using Home-Made Disperse agent in making slurry
Solid content can only accomplish 55%-59%, and use A-15, and solid content normally accomplishes 63%-65%, and when so granulating, moisture content steams
The hair time is short, and Ion transfer is few) make slurry fluidity more preferably, it is easy to the crushing and mixing of powder.
In order to detect the made performance for carrying product of the inventive method, tight aging examination is added to piezoresistor design equivalent simulation
Test.
Piezoresistor is also that main failure mode is about the ageing failure pattern of stability:Deterioration, piezo-resistance
Device is in length
In the case of phase hot and humid energization, only a few, several product of ten thousand/several or even hundreds of thousands point can show as
Leakage current
Increase, pressure sensitive voltage declines, long-term in the past until being zero;So as to cause product to puncture.
According to above failure mode, we have formulated many degradation harsher than standard, double 85 experiments, i.e., in temperature
It it is 85 degree, relative humidity is maximum continuously DC voltage 1000 hours of applying under conditions of 85%RH.Performance leakage current after experiment
Less than 10 microamperes.Product has passed through this experiment, and its stability, reliability are greatly improved.
The present invention improves raw material, is formulated adjustment, increases Ball-milling Time, increase product safety surplus, makes product stabilization
Property greatly improve, by improving before user using have within 1 year it is several ageing failure complain, had using 1 year to the user after improving
Complained without ageing failure;After direct current ceiling temperature endurancing 1000 hours before by improving, leakage current is generally micro- 10.0
More than peace, after the direct current ceiling temperature endurancing 1000 hours to after improving, leakage current is generally below 3.0 microamperes.
Before improvement, piezoresistor is used, there are several every year, be concentrated mainly on summer, because piezoresistor loses
Imitate and cause to complain, equipment is stopped after typically burning circuit board, and fire is caused sometimes.Do not go out after after the process modification
The situation for burning circuit board together is now crossed, not to mention causes fire.The stabilisation of piezoresistor is improved and substantially increases pressure
The reliability that sensitive resistor is used.
Specific embodiment
Embodiment 1:High stability zinc oxide varistor makes
Carry out according to the following steps:
Dispensing:Various chemical raw material compositions are weighed by formula, is calculated as by weight:Zinc oxide 100000g, three oxidations
Two bismuth 3400g, antimony oxide 3500g, cobaltosic oxide 1400g, chrome green 240g, nickel sesquioxide 600g, oxidation
Manganese 520g, silver-colored glass powder 100g.
Ball milling:By deionized water, deflocculant A-15 dispersants (purchasing from Taixing Dong Jin chemical plant), adhesive and weighing
Good chemical raw material successively pours into milling system ball milling 6 hours.
Granulation:Slow the stirring in bucket that mist projection granulating is put into after the good slurry sieving of ball milling is stirred, and is granulated by granulation tower.
Shaping:The dimensions and pressure that granulation material is specified by description of the process are pressed into required green compact.
Sintering:Green compact are pressed into technological requirement dumping heel row in saggar is sintered, by the temperature and curve negotiating of process stipulation
Tunnel kiln sintering.By the way of sintering temperature is adjusted again after prerun burning, control pressure sensitive voltage scope is -2% to+10%.
Electrode processed:Low temperature silver paste and silver ink firing on ceramics perfecting.
Welding encapsulating:Silver strip is burn-on lead-out wire, and wraps epoxy powder.Product is obtained.
According to above-mentioned steps elder generation small lot, middle batch, produce in enormous quantities again, while full performance test is done every time, especially
Concern upper category temperature durability, peak inrush current experiment, as a result three times it is qualified.
On upper category temperature endurance issues:
It is exactly the embodiment of upper category temperature endurancing in view of aging, stability problem, goes back emphasis and done following
Work:
1. strengthen the control of deionized water quality, checked in addition to water resistance when factory is entered, check water resistance, water resistance to be less than 1M before dispensing
Ω must scrap, it is impossible to use.
2. production process control is strengthened, in whole product operation process, hand is unable to directly contact product, it is necessary to band
Gloves are operated.
3. Control Welding Process is carried out.Welding temperature could be welded in prescribed limit, every batch of material test weld three, and inspection is closed
Could batch welding after lattice.Operating personnel, inspector perform first inspection, patrol and examine work.Waster statistic record, solder flux are carried out per batch of material
Thermograph.
4. test leakage current includes me and takes charge of product routine test category after this is tested.
5. sintering ceramics with running water after being cleaned, then is cleaned with deionized water one time, harmful miscellaneous in reduction running water
The influence of confrontation product.
6. the cleaning solvent after Product jointing is changed.The industrial grade ethanol that will originally use is replaced by dissolubility
More preferable solvent, it is pure that purity rises to chemistry, preferably can wash welding residual flux, and seldom bring new dirt into
Dye.
Claims (5)
1. a kind of high stability zinc oxide varistor preparation method, including dispensing, ball milling, granulation, shaping, sintering, system electricity
The step of pole and welding encapsulating, it is characterised in that:In batching step, the d50 of the zinc oxide of use below 0.4 micron, other
Doping material bismuth oxide, antimony oxide, cobaltosic oxide, chrome green, nickel sesquioxide, manganese oxide are existed using d50
The raw material of less than 1.0 microns and purity more than 99.7%.
2. method according to claim 1, it is characterised in that the Ball-milling Time of ball milling step is 6 hours.
3. method according to claim 1, it is characterised in that in batching step, the content of silver-colored glass powder is oxidation in formula
The 0.1% of zinc;Chromic oxide content is the 0.24% of zinc oxide.
4. method according to claim 1, it is characterised in that dispersant is made using deflocculant A-15 in ball milling step.
5. method according to claim 1, it is characterised in that adjust sintering temperature again after being burnt using prerun in sintering step
Mode, control pressure sensitive voltage scope in -2%-+10%.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109065305A (en) * | 2018-06-28 | 2018-12-21 | 南京先正电子股份有限公司 | A kind of band two temperature insurance piezoresistor and preparation method thereof |
CN114360829A (en) * | 2021-11-30 | 2022-04-15 | 南京先正电子股份有限公司 | Large-through-flow-capacity moisture-resistant voltage-sensitive resistor for electric meter and preparation method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109065305A (en) * | 2018-06-28 | 2018-12-21 | 南京先正电子股份有限公司 | A kind of band two temperature insurance piezoresistor and preparation method thereof |
CN114360829A (en) * | 2021-11-30 | 2022-04-15 | 南京先正电子股份有限公司 | Large-through-flow-capacity moisture-resistant voltage-sensitive resistor for electric meter and preparation method thereof |
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