CN107705946A - A kind of high-pass flow zinc oxide resistor sheet and its production technology - Google Patents
A kind of high-pass flow zinc oxide resistor sheet and its production technology Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- 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
- H01C7/105—Varistor cores
- H01C7/108—Metal oxide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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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- C04B35/62605—Treating the starting powders individually or as mixtures
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- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- 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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Abstract
The present invention relates to high pressure electrician's ceramic material sensitive to heat-humidity technical field, a kind of high-pass flow zinc oxide resistor sheet and its production technology are disclosed.Wherein, a kind of high-pass flow zinc oxide resistor sheet of the invention, including zinc oxide, bismuth oxide, cobalt sesquioxide, nickel sesquioxide, manganese sesquioxide managnic oxide, antimony oxide, silica, glass dust and aluminum nitrate.In the high-pass flow zinc oxide resistor sheet formula of the present invention, close to 1, sintering forms Zn for antimony and silicone content ratio7Sb2O12、ZnSiO4And preferably ratio distribution, so as to reach the purpose of the electric potential gradient and current density that improve zinc oxide resistance sheet.Meanwhile high-pass flow zinc oxide resistor sheet of the invention, selected additive ball milling complexity is reasonable, simplifies ball-milling technology, and the selection to Ball-milling Time is optimized, and controls ball milling hybrid technique make it that the zinc oxide resistance sheet raw material particle size after ball milling is small and uniform.
Description
Technical field
The present invention relates to high pressure electrician's ceramic material sensitive to heat-humidity technical field, more particularly, to a kind of high throughflow zinc oxide
Resistor disc and its production technology.
Background technology
Zinc oxide resistance sheet is the core component of operation of power networks protection equipment metal oxide arrester, is higher by just when running into
When the lightning surge or switching overvoltage of normal voltage manyfold attack, the resistance value of zinc oxide resistance sheet can be instantaneously by high resistance
Turn to low resistance, the oxidized zinc resistor disc of powerful momentary excess current is flowed into the earth, so as to avoid electrical equipment by
Voltage attacks and influences electric power netting safe running, so far, the installation metal oxidation series-parallel with insulator on transmission line of electricity
Thing arrester is considered to prevent one of most effective means of lightning stroke trip always.
In recent years, line arrester with gaps is largely installed on the line, is effectively reduced circuit accumulation trip-out rate, is disappeared
Except insulator surface damages caused by lightning stroke flashover.But at present, conventional zinc oxide resistance sheet gradient be 2000~
2200V/cm, rectangular surge discharge current density only 20~22A/cm2, arrester with gaps structure height is usually more exhausted than same voltage class circuit
Edge it is long 20 parts and more than, volume, weight, cost depend on resistor disc through-current capability, and the through-current capability of resistor disc is not strong at present,
Cause existing line arrester big and weigh, installation and maintenance are extremely inconvenient, and extensive use is affected on the line for it.I
State's high-potential gracient and the demand of strong through-current capability zinc oxide resistance sheet rely primarily on external import, are not formed to possess and independently known
Know the formula and production technology of property right, it is expensive.As what the development of China's power network, transmission line of electricity operational reliability required carries
Demand that is high and reducing manual maintenance cost, line is reduced to the zinc oxide resistance sheet using high-potential gracient, strong through-current capability
Road arrester height, volume, weight and cost, meet that line thunder protection demand is increasingly urgent.
In order to develop the high performance line arrester for meeting service requirement, being easily installed, safeguarding, China's transmission line of electricity is improved
Overall lightning protection it is horizontal, be badly in need of developing a kind of high-potential gracient for lowering leakage conductor structure height and strong through-current capability
ZnO varistor formula and and its processing technology.
The content of the invention
The present invention provides a kind of high-pass flow zinc oxide resistor sheet and its processing technology, to solve upper existing zinc oxide resistance sheet
Through-current capability it is not strong, caused existing line arrester is big and weigh, installation and safeguards the extremely technical problem of inconvenience.
According to an aspect of the present invention, there is provided a kind of high-pass flow zinc oxide resistor sheet, in parts by weight, by including as follows
Raw material is made：Zinc oxide is 85~90 parts, and bismuth oxide is 2.5~3.5 parts, and cobalt sesquioxide is 2~3 parts, three oxidations two
Nickel be 0.6~0.7 part, manganese sesquioxide managnic oxide be 0.3~0.35 part, antimony oxide be 3.5~4.0 parts, silica be 1.4~
1.6 parts, glass dust is 0.15~0.25 part, and aluminum nitrate is 0.05~0.1 part.
On the basis of such scheme preferably, a kind of high-pass flow zinc oxide resistor sheet of the invention, in parts by weight, by including
The following raw material is made：Zinc oxide be 88~89 parts, bismuth oxide be 2.5~3 parts, cobalt sesquioxide be 2.3~2.5 parts, three
Two nickel are aoxidized as 0.6~0.7 part, manganese sesquioxide managnic oxide is 0.3~0.35 part, and antimony oxide is 2.3~2.5 parts, silica
For 1.4~1.6 parts, glass dust is 0.2~0.25 part, and aluminum nitrate is 0.05~0.1 part.
On the basis of such scheme preferably, the side surface of the zinc oxide resistance sheet is provided with resistive formation, the resistive formation
Raw material is powder, alcohol, dibutyl phthalate, the mixture of ethyl cellulose.
On the basis of such scheme preferably, the powder in parts by weight, including the following raw material：Zinc oxide is 14~17.0
Part, oxidation two bismuths be 25~30 parts, antimony oxide be 40~45 parts, titanium oxide be 15~17 parts, lithium carbonate be 0.24~
0.36 part.
Preferably, when the powder in parts by weight, including the following raw material：Zinc oxide is 15.7 parts, and two bismuths of oxidation are 26
Part, antimony oxide is 42 parts, and titanium oxide is 16 parts, and when lithium carbonate is 0.3 part, its insulating properties is more preferable.
On the basis of such scheme preferably, the glass dust in parts by weight, by including the following raw material：Boron oxide is 14.5
Part, zinc oxide is 42 parts, and silica is 26 parts, and two bismuths of oxidation are 17.5 parts.
On the basis of such scheme preferably, the zinc oxide resistance sheet is made by the raw material through ball milling, sintering；Wherein,
The ball milling is specially：By 180~240min of other raw material ball millings in addition to zinc oxide, zinc oxide and water, glue are added thereto
Body grinds 270~360min；Preferably, by other raw material ball milling 210min in addition to zinc oxide, zinc oxide and water are added thereto,
Colloid mill 300min.
On the basis of such scheme preferably, the sintering step includes pre-sintered and double sintering, described pre-sintered specific
For：The zinc oxide resistance sheet preform is carried out pre-sintered, obtains the pre- semi-finished product of zinc oxide resistance sheet, and it is described it is pre-sintered most
High-temperature is 760~770 DEG C.
On the basis of such scheme preferably, the double sintering：The pre- semi-finished product of zinc oxide resistance sheet are subjected to double sintering,
To obtain zinc oxide resistance sheet semi-finished product, and the maximum temperature of the double sintering is 1050 ± 10 DEG C.
Present invention also offers a kind of production technology of high-pass flow zinc oxide resistor sheet, comprise the following steps：
S1. raw material is prepared, and adhesive is added in the raw material of the zinc oxide resistance sheet and water carries out ball milling mixing, with
To 1 μm~2 μm of particle diameter of discharging, viscosity is 40~90MPas, and the slurry of 40~65 parts of slurry solid content；
S2. drying-granulating：By the slurry obtained by step S1 by granulating and drying tower with drying-granulating, and shaken through 100 mesh
Dynamic sieve, to obtain granulation material of the moisture content as (0.4 ± 0.1) part；
S3. it is dry-pressing formed：Granulation material is pressed into the zinc oxide resistance sheet preform of preset shape, the ZnO resistors
The density of piece meets ρ=(3.15 ± 0.05) g/cm3；
S4. sinter：The zinc oxide resistance sheet preform is sintered, obtains zinc oxide resistance sheet semi-finished product；
S5. it is electrode coated：In the electrode coated slurry of upper and lower surface of the zinc oxide resistance sheet semi-finished product, oxygen is obtained after firing
Change zinc resistor disc.
On the basis of such scheme preferably, the raw material, which is prepared, includes additive preparation, adhesive is prepared, aluminum nitrate solution
Preparation and slurry preparation.
On the basis of such scheme preferably, the additive is prepared and comprised the following steps, and is aoxidized according to formula rate by three
Two bismuths, cobalt sesquioxide, nickel sesquioxide, manganese sesquioxide managnic oxide, antimony oxide, silica and glass dust add stirring ball-milling
In machine, add water mixing 210min, and mixed liquor crossed into 300 mesh with upper screen cloth in case with.
On the basis of such scheme preferably, described adhesive is prepared and specifically included, and water is added in glue machine is changed, and adjusts water temperature
To 60 DEG C, polyvinyl alcohol and dispersant are added, regulation water temperature is incubated 30min to more than 90 DEG C.
On the basis of such scheme preferably, the slurry preparation specifically includes following steps, and water is added in high agitator tank
And adhesive, stirring at low speed 5min, the zinc oxide of formula rate is added, 10min is stirred and adds additive and aluminum nitrate solution,
Stir, start colloid mill and circulating pump, colloid mill 300min, to obtain 1 μm~2 μm of the particle diameter that discharges, viscosity is 40~
90MPas, and the slurry of 40~65 parts of slurry solid content.
On the basis of such scheme preferably, it is described dry-pressing formed preceding also including granulation material and water are added into batch mixing tank containing water dispenser
Interior, it is 1.2 ± 0.3 parts to control the moisture content in granulation material, wherein, amount of water is 1.2 parts of material gross weight.
On the basis of such scheme preferably, the sintering step includes pre-sintered and double sintering, wherein, the pre-burning
Knot：The zinc oxide resistance sheet preform is subjected to pre-sintering, obtains the pre- semi-finished product of zinc oxide resistance sheet, and the pre-sintered highest temperature
Spend for 760~770 DEG C；
The double sintering：The pre- semi-finished product of zinc oxide resistance sheet are subjected to double sintering, to obtain zinc oxide resistance sheet half
Finished product, and the maximum temperature of the double sintering is 1050 ± 10 DEG C.
On the basis of such scheme preferably, the pre-sintering concretely comprises the following steps：First the zinc oxide resistance sheet preform is put
Kiln is put, the temperature of kiln is continuously risen to 400 DEG C in 16h, then, is incubated 4h every time, kiln temperature is raised 100 every time
DEG C, until temperature rises to 760~770 DEG C, soaking time 12h, then ladder is cooled to 560 DEG C of insulation 4h, then is cooled to 420
DEG C, kiln discharge, normal temperature is naturally cooled to, to obtain obtaining the pre- semi-finished product of zinc oxide resistance sheet.
On the basis of such scheme preferably, the double sintering concretely comprises the following steps：The pre- semi-finished product of initial oxidation zinc resistor disc are put
Kiln is put, the temperature of kiln is continuously risen to 800 DEG C ± 10 DEG C in 16h, is incubated 18h, then, temperature is risen to 920, insulation
8h, then temperature is risen to 1050 DEG C ± 10 DEG C, 16~17h of soaking time, 870 DEG C of insulation 4h are then cooled to, are then cooled again
760 DEG C, kiln discharge, normal temperature is naturally cooled to, to obtain obtaining zinc oxide resistance sheet semi-finished product.
On the basis of such scheme preferably, resistive formation coating process is provided between the pre-sintered and double sintering, passed through
Resistive formation slurry is brushed to the side of the pre- semi-finished product of zinc oxide resistance sheet by coating machine.
Compared with prior art, the advantage of the invention is that：
1. the high-pass flow zinc oxide resistor sheet of the present invention, selected additive ball milling complexity is reasonable, simplifies ball milling work
Skill, the selection to Ball-milling Time are optimized, and control ball milling hybrid technique to cause the ZnO resistors tablet raw material after ball milling
Particle diameter is small and uniform.
2. in the high-pass flow zinc oxide resistor sheet formula of the present invention, close to 1, sintering is formed for antimony and element silicon molar content ratio
Zn7Sb2O12、ZnSiO4And preferably ratio distribution, so as to reach the electric potential gradient and current density of raising zinc oxide resistance sheet
Purpose.Because the double sintering temperature of the present invention is not higher than 1100 DEG C, Bi is reduced2O3Volatilization, improve the cause of resistor disc
Close property.
3. the high-pass flow zinc oxide resistor sheet that the present invention develops, during for leakage conductor, its resistor disc total length used
35% can be reduced, arrester with gaps total length can be reduced by 20% or so, volume suitable with common insulator length
Declined to a great extent with weight, it is convenient for installation and maintenance, due to resistance sheet material be reduced to it is original less than half, product qualified rate reaches
To 95.20 parts, cost will also be greatly reduced.
Brief description of the drawings
The high-energy ball milling that Fig. 1 is the present invention prepares distribution of particles figure of the zinc oxide after 1050 DEG C of sintering；
Fig. 2 is the pre-sintering temperature curve map of the present invention；
Fig. 3 is the double sintering temperature profile of the present invention；
Fig. 4 is the heat treatment temperature curve map of the present invention；
Fig. 5 is the degradation change of power consumption curve map of the present invention；
Fig. 6 is the blank scanning electronic microscope observation figure of the dry-pressing formed rear high-pass flow zinc oxide resistor sheet of the present invention；
Fig. 7 is the pictorial diagram of the ring-like high-pass flow zinc oxide resistor sheet of the present invention；
The manufacturing process flow diagram of the high-pass flow zinc oxide resistor sheet of Fig. 8 present invention.
Embodiment
With reference to the accompanying drawings and examples, the embodiment of the present invention is described in further detail.Implement below
Example is used to illustrate the present invention, but is not limited to the scope of the present invention.
The invention provides a kind of high-pass flow zinc oxide resistor sheet, in parts by weight, by being made including the following raw material：Oxidation
Zinc is 85~90 parts, and bismuth oxide is 2.5~3.5 parts, and cobalt sesquioxide is 2~3 parts, and nickel sesquioxide is 0.6~0.7
Part, manganese sesquioxide managnic oxide is 0.3~0.35 part, and antimony oxide is 3.5~4.0 parts, and silica is 1.4~1.6 parts, glass dust
For 0.15~0.25 part, aluminum nitrate is 0.05~0.1 part.
A kind of high-pass flow zinc oxide resistor sheet of the present invention, by adding cobalt sesquioxide in zinc oxide to improve resistance
Piece nonlinear characteristic, increase energy density and barrier height is improved, add nickel sesquioxide to improve zinc oxide resistance sheet can
By property, stability and aging characteristics are exchanged, coordinate the bismuth oxide of addition to promote liquid-phase sintering.
Preferably, a kind of high-pass flow zinc oxide resistor sheet of the invention, in parts by weight, by being made including the following raw material：
Zinc oxide is 88~89 parts, and bismuth oxide is 2.5~3 parts, and cobalt sesquioxide is 2.3~2.5 parts, nickel sesquioxide 0.6
~0.7 part, manganese sesquioxide managnic oxide is 0.3~0.35 part, and antimony oxide is 3.5~4.0 parts, and silica is 1.4~1.6 parts,
Glass dust is 0.2~0.25 part, and aluminum nitrate is 0.05~0.1 part.
It should be noted that the high-pass flow zinc oxide resistor sheet of the present invention is in annular, as shown in fig. 7, in order to improve oxidation
The side insulation performance of zinc resistor disc, the present invention are also provided with resistive formation in the side surface of zinc oxide resistance sheet, wherein, resistive formation is
Resistive formation slurry is formed through three roller ball mill ball milling mixings by powder, alcohol, dibutyl phthalate, ethyl cellulose, is led to
Cross coating machine and slurry is brushed to coating of the zinc oxide resistance sheet blank side drying to be formed, what deserves to be explained is the present invention
Powder, alcohol, dibutyl phthalate, the proportioning of ethyl cellulose are：65g:65ml:4ml:5g.
Wherein, powder of the invention in parts by weight, including the following raw material：Zinc oxide is 14~17.0 parts, aoxidizes two bismuths
For 25~30 parts, antimony oxide is 40~45 parts, and titanium oxide is 15~17 parts, and lithium carbonate is 0.24~0.36 part.
Preferably, when the present invention powder in parts by weight, including the following raw material：Zinc oxide is 15.7 parts, aoxidizes two bismuths
For 26 parts, antimony oxide is 42 parts, and titanium oxide is 16 parts, and lithium carbonate is 0.3 part, and its insulation effect is more preferable.
Refer to shown in Fig. 7, glass dust of the invention in parts by weight, by being made including the following raw material：Boron oxide is
14.5 parts, zinc oxide is 42 parts, and silica is 26 parts, and two bismuths of oxidation are 17.5 parts.
Present invention also offers a kind of production technology of high-pass flow zinc oxide resistor sheet, comprise the following steps：
S1. raw material is prepared, and adhesive is added in the raw material of zinc oxide resistance sheet and water carries out ball milling mixing, to be gone out
Expect 1 μm~2 μm of particle diameter, viscosity is 40~90MPas, and the slurry of 40~65 parts of slurry solid content；
S2. drying-granulating：By the slurry obtained by step S1 by granulating and drying tower with drying-granulating, and shaken through 100 mesh
Dynamic sieve, to obtain granulation material of the moisture content as (0.4 ± 0.1) part；
S3. it is dry-pressing formed：Granulation material is pressed into the zinc oxide resistance sheet preform of preset shape, the ZnO resistors
The density of piece meets ρ=(3.15 ± 0.05) g/cm3；
S4. sinter：The zinc oxide resistance sheet preform is sintered, then in side brushing resistive formation, carries out two
After secondary sintering, zinc oxide resistance sheet semi-finished product are obtained；
S5. it is electrode coated：In the electrode coated slurry of upper and lower surface of the zinc oxide resistance sheet semi-finished product, oxygen is obtained after firing
Change zinc resistor disc.
In another preferred embodiment of the present invention, raw material of the invention, which is prepared, includes additive preparation, adhesive is prepared,
Aluminum nitrate solution is prepared and slurry preparation.
Wherein, additive is prepared and comprised the following steps, and according to formula rate, is claimed successively with the scoop of cleaning, electronic balance
Bismuth oxide, cobalt sesquioxide, nickel sesquioxide, manganese sesquioxide managnic oxide, antimony oxide, silica and glass dust is taken to load
In special batching bucket, after treating that whole additives weigh, electronic scale verifies that the gross weight of each tubbing should be with each part sum phase
Symbol, the additive raw material in mixer is added in agitating ball mill, add 5L water, and cover tightly lid, start agitating ball mill
Button, ball milling 210min, agitating ball mill 300~500r/min of rotating speed, and according to rotating forward 30min, reversion 30min alternately and repeatedly
Ball milling, and it is standby with upper screen cloth that mixed liquor is crossed into 300 mesh.It should be noted that bismuth oxide, three oxygen in inventive formulation
It is by single substance ball milling to change two cobalts, nickel sesquioxide, manganese sesquioxide managnic oxide, antimony oxide, silica and glass dust
Therefore 80min~100min, can effectively ensure each to obtain, and because the ball milling complexity of each compound is approximate
The particle diameter of compound is kept in 1 μm~2 μ ms, so as to ensure that the even particle size of raw material is consistent.Meanwhile in ball
During mill, in order to be further ensured that additive even particle size is consistent and the uniformity of final slurry, present invention employs
High energy ball carries out ball milling.As shown in figure 1, be the present invention zinc oxide under different time, different size of Zinc oxide particles number
Measure the Zinc oxide particles diameter graph of a relation after percentage when sinters at 1050 DEG C.
Wherein, adhesive of the invention is prepared and specifically included, and 10L water is added in glue machine changing, when water temperature is risen into 60 DEG C,
Starting agitator operating, polyvinyl alcohol and dispersant are added in glue machine to changing, water temperature rises to more than 90 DEG C, is incubated more than 30min,
To ensure that solution is transparent, no sheet, pellet shape polyvinyl alcohol are remaining, standby.
And the method that the aluminum nitrate solution of the present invention is prepared is that, according to formula, weighing aluminum nitrate pours into stainless steel cup, add
Enter pure water 100mL, stirred with insulating bar, it is standby.
It should be noted that the additive of the present invention is prepared, adhesive is prepared, aluminum nitrate solution is prepared simultaneously to enter
OK, can also successively carry out.
When additive is prepared, adhesive is prepared, aluminum nitrate solution is prepared after all preparing, wherein slurry preparation.And this
The slurry preparation of invention specifically includes following steps, addition 10L water and adhesive in high agitator tank, stirring at low speed 5min, then
40kg zinc oxide is added, adds 100mL defoamers after stirring 5min, adjustment mixing speed is high-speed stirred, after being stirred for 5min
Additive and aluminum nitrate solution are added, is stirred, starts colloid mill and circulating pump, colloid mill 300min, to obtain the grain that discharges
1 μm~2 μm of footpath, viscosity are 40~90MPas, and the slurry of 40~65 parts of slurry solid content.
Further, drying-granulating detailed step of the invention is：By the slurry that stirs in tank of height squeeze into it is low stir in tank, will make
To 170~220 DEG C, air pressure is adjusted to 1.8MPa, the regulation of hothouse static pressure grain tower drying-granulating air heater, and is kept
Hothouse range of negative pressure is in -5~+10mmH2Change in O, stirred slurry in tank by low with spray gun and sprayed to granulation tower hothouse,
Then granulation material is crossed into 100 mesh vibratory sieves.
Slurry beat to it is low stir tank when, to ensure the uniformity of granulation material and density, prevent granulation tower glues from wall and having been formed
Spherical grain secondary agglomeration, control slurry meet：Viscosity is 40~90MPas；Solid content is 40~65 parts；And slurry temperature
Control is at 55~70 DEG C.
Complete after being granulated, granulation material is inspected by random samples, it is desirable to granulation material color uniformity；Moisture content scope (0.4 ±
0.1) in part.
Preferably, occurring lamination in order to prevent during dry-pressing formed, inside zinc oxide resistance sheet influences its property
Can, the present invention also it is dry-pressing formed it is preceding be provided with following steps, i.e., by granulation material and water addition batch mixing tank containing water dispenser in, by air pressure
Power is adjusted to 0.4MPa, pre- do time of setting is set as 5min for 2min, humidification periods, and the accumulative aqueous time is set as 23min.
Granulation material is added in batch mixing feeding engine tank and covers tightly cover plate, pure water is added into batch mixing feeding engine water tank, amount of water is material
1.2 parts of gross weight.It is aqueous to finish, water cut test is carried out to aqueous material by technique person, the moisture content for controlling water granulation material is：
(1.2 ± 0.3) part.
The dry-pressing formed concrete technology of the present invention is：Aqueous granulation material is added into hopper, first pressure testing, makes blank density
Meet ρ=(3.15 ± 0.05) g/cm3, the pressing pressure of press is determined according to density size, then sets the maximum pressure of tablet press machine
Power, exhaust number is set as 3 times, evacuation time is 6 seconds and 10 seconds dwell times, opens automatic running button, makes it from dynamic pressure
Piece.It is Φ 85mm (external diameter)/Φ 26mm (internal diameter)/22mm (thickness) to obtain the size of resistor disc, base when dry-pressing formed
The external diameter of piece is 104.9 ± 0.5mm of Φ, and the internal diameter of the blank is 31.9 ± 0.5mm of Φ, and thickness is 28.5 ± 0.5, will be suppressed
Good blank brushes away flash with hairbrush.
And explanation is made, sintering step of the invention includes pre-sintered and double sintering, wherein, it is pre-sintered：By oxygen
Change zinc resistor disc preform and carry out pre-sintered, obtain the pre- semi-finished product of zinc oxide resistance sheet, and pre-sintered maximum temperature for 760~
770℃。
Concrete operations mode is：Initial oxidation zinc resistor disc preform is placed in kiln, by the temperature of kiln in 16h it is continuous
400 DEG C are risen to, then, after being incubated 4h every time, kiln temperature is gradually raised 100 DEG C, until temperature rises to 760~770 DEG C, protected
Warm time 12h, then ladder is cooled to 560 DEG C of insulation 4h, then is cooled to 420 DEG C, kiln discharge, normal temperature is naturally cooled to, to obtain
The pre- semi-finished product of zinc oxide resistance sheet are obtained, control the shrinkage factor of the pre- semi-finished product of zinc oxide resistance sheet within 8.5 parts~11.5 parts.Its
In, the controlling curve of pre-sintering temperature of the invention and time, refer to shown in Fig. 2.
Double sintering：The pre- semi-finished product of zinc oxide resistance sheet are subjected to double sintering, to obtain zinc oxide resistance sheet semi-finished product,
And the maximum temperature of the double sintering is 1050 ± 10 DEG C.
Wherein, double sintering concretely comprises the following steps：The pre- semi-finished product of initial oxidation zinc resistor disc place kiln, and the temperature of kiln is existed
800 DEG C are continuously risen in 16h, is incubated 18h, then, temperature is risen to 920, is incubated 8h, then temperature is risen to 1050 DEG C, insulation
16~17h of time, be then cooled to 870 DEG C insulation 4h, then cool again 760 DEG C, kiln discharge, naturally cool to normal temperature, take out with
Obtain obtaining zinc oxide resistance sheet semi-finished product.The litter particle of zinc oxide resistance sheet surface of semi-finished adhesion is removed, electricity is carried out to it
Performance test, hair piece point potential gradient control is in the range of 250~300V/mm, the μ A of leakage current parameter≤10.Wherein, it is of the invention
Double sintering temperature and time controlling curve, refer to shown in Fig. 3.
As another preferred embodiment of the present invention, the present invention is provided with resistive formation between pre-sintered and double sintering and is coated with
Technique, to improve the side insulation performance of zinc oxide resistance sheet, concrete operation step is：Using resistive formation powder, alcohol, adjacent benzene
Dibutyl carboxylic acid, ethyl cellulose form resistive formation slurry through three roller ball mill ball milling mixings, are applied slurry by coating machine
Blank side is brushed, blank side slurry answers thickness uniform, and edge is equal with resistor disc both ends.Coated blank interval is uniform
Ground is placed in stainless steel Dropbox, naturally dry.
As another preferred embodiment of the present invention, electrode coated concrete operation step of the invention is：In zinc oxide
The electrode coated slurry of upper and lower surface of resistor disc semi-finished product, zinc oxide resistance sheet is obtained after firing.Use full-automatic zinc oxide valve
The aluminium-plated machine of piece, aluminum electrode slurry is coated to the resistor disc upper and lower surface that need to be sprayed, the resistor disc sprayed is removed with nylon bruss
End face aluminium skimmings, the aluminum shot of side bonding is removed with sand paper, is then blown clean with gas.
Finally, the zinc oxide resistance sheet after will be electrode coated carries out the glaze coating of low temperature side.Cleaned with alcohol by coating electricity
The floating ash of Zinc-oxide resistor-piece side after extremely, using coating machine, by the low temperature side glaze slurry to stir to resistor-piece side
It is coated twice, side glaze answers thickness uniform, and edge is equal with resistor disc both ends.Coated resistor disc should be evenly and at intervals
1~the 2h that dries in the air is placed in stainless steel Dropbox, is then placed in baking oven and is solidified, oven temperature is set as 150 ± 30 DEG C, insulation
Time is set as 70 ± 30min.
Further, the present invention also it is electrode coated it is preceding also carried out grinding cleaning and heat treatment two steps.Wherein, it is first
First valve block end face is polished using double-ended grinding machine, and cleaned up with running water, the resistor disc after cleaning is placed in back
Turn tunnel cave carries out heat treatment 15min, and it is 600 DEG C that highest, which controls temperature,.Then the zinc oxide resistance sheet after being cleaned to grinding
It is heat-treated, the zinc oxide resistance sheet after will cleaning is placed in evenly and at intervals to be burnt in alms bowl, is placed in entering for revolution tunnel cave
Row heat treatment 15min, it is 600 DEG C that highest, which controls temperature, wherein, heat treatment temperature curve such as Fig. 4.
In order to verify the effect of the zinc oxide resistance sheet of the present invention, it is Φ 85mm/ Φ to produce specification according to aforesaid way
26mm/22mm ring-like zinc oxide resistance sheet zinc oxide resistance sheet, rushed using 2ms/1650A square waves and 20kA, 8/20 μ s thunders and lightnings
Screening is hit, qualification rate is up to 95.20 parts.Extract 10 sheet resistance pieces survey its gradient and using 1650A square wave currents carry out 18 times it is resistance to
It is put to the test, as a result such as table 1, wherein in table 1, U1mAVoltage of the resistor disc by both ends during direct current 1mA electric currents is represented, claims direct current
1mA voltages or pressure sensitive voltage, 0.75U1mAVoltage of the resistor disc by both ends during direct current 0.75mA electric currents is represented, claims direct current
0.75mA voltages or pressure sensitive voltage.As shown in Table 1, the zinc oxide small electric bulb piece point potential gradient of the present embodiment may be up to 271V/mm, and
In 1650A, 2ms square waves tolerance number is 18 times, and its square wave through-current capability is 32.1A/cm2, the maximum reference under rectangular impulse
Voltage range is 8.53-8.73KV.
The Φ 85mm/ Φ 26mm/22mm of table 1 ring-like zinc oxide resistance sheet gradient and square wave current test data
Choose 3 sheet resistance pieces and carried out high-temperature circulation test, typical degradation curve is shown in Fig. 5, aging temperature 135
DEG C, application voltage is 4.5kV, and highest power consumption is 13W, lowest power consumption 8.18W, ageing time 187.7h, stable performance.
Compared with prior art, the advantage of the invention is that：
1. the high-pass flow zinc oxide resistor sheet of the present invention, selected additive ball milling complexity is reasonable, simplifies ball milling work
Skill, the selection to Ball-milling Time are optimized, and control ball milling hybrid technique to cause the ZnO resistors tablet raw material after ball milling
Particle diameter is small and uniform, as shown in fig. 6, for the zinc oxide resistance sheet blank after the dry shaping of the present invention under a scanning electron microscope
Observation chart, actual measurement particle diameter is usually no more than 5 μm after sintering in figure, and median is about 2.5 μm；
2. in the high-pass flow zinc oxide resistor sheet formula of the present invention, close to 1, sintering forms for antimony and silicone content ratio
Zn7Sb2O12、ZnSiO4And preferably ratio distribution, so as to improve the electric potential gradient and current density of zinc oxide resistance sheet to reach
Purpose.Because the double sintering temperature of the present invention is not higher than 1100 DEG C, Bi is reduced2O3Volatilization, improve the densification of resistor disc
Property.
3. the high-pass flow zinc oxide resistor sheet that the present invention develops, during for leakage conductor, its resistor disc total length used
35 parts can be reduced, arrester with gaps total length can be reduced by 20 parts or so, volume suitable with common insulator length
Declined to a great extent with weight, it is convenient for installation and maintenance, due to resistance sheet material be reduced to it is original less than half, product qualified rate reaches
To 95.20 parts, cost will also be greatly reduced.
Finally, the present processes are only preferable embodiment, are not intended to limit the scope of the present invention.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements made etc., the protection of the present invention should be included in
Within the scope of.
Claims (10)
1. a kind of zinc oxide resistance sheet, it is characterised in that in parts by weight, by being made including the following raw material：Zinc oxide be 85~
90 parts, bismuth oxide is 2.5~3.5 parts, and cobalt sesquioxide is 2~3 parts, and nickel sesquioxide is 0.6~0.7 part, three oxidations
Two manganese be 0.3~0.35 part, antimony oxide be 3.5~4.0 parts, silica be 1.4~1.6 parts, glass dust be 0.15~
0.25 part, aluminum nitrate is 0.05~0.1 part.
2. a kind of zinc oxide resistance sheet as claimed in claim 1, it is characterised in that the zinc oxide is 88~89 parts, described
Cobalt sesquioxide is 2.3~2.5 parts.
3. a kind of zinc oxide resistance sheet as claimed in claim 1, it is characterised in that the side surface of the zinc oxide resistance sheet is set
There is resistive formation, the raw material of the resistive formation is powder, alcohol, dibutyl phthalate, the mixture of ethyl cellulose.
A kind of 4. zinc oxide resistance sheet as claimed in claim 3, it is characterised in that the powder in parts by weight, including such as
Lower raw material：Zinc oxide is 14~17.0 parts, and two bismuths of oxidation are 25~30 parts, and antimony oxide is 40~45 parts, titanium oxide 15
~17 parts, lithium carbonate is 0.24~0.36 part；Preferably, the powder in parts by weight, including the following raw material：Zinc oxide is
15.7 parts, two bismuths of oxidation are 26 parts, and antimony oxide is 42 parts, and titanium oxide is 16 parts, and lithium carbonate is 0.3 part.
5. a kind of zinc oxide resistance sheet as claimed in claim 1, it is characterised in that the zinc oxide resistance sheet is by the raw material
It is made through ball milling, sintering；Wherein, the ball milling is specially：By 180~240min of other raw material ball millings in addition to zinc oxide, to
Wherein add zinc oxide and water, 270~360min of colloid mill；Preferably, by other raw material ball milling 210min in addition to zinc oxide,
Zinc oxide and water, colloid mill 300min are added thereto.
6. a kind of zinc oxide resistance sheet as claimed in claim 5, it is characterised in that the sintering includes pre-sintered and secondary burning
Knot, the pre-sintering are specially：The zinc oxide resistance sheet preform is carried out it is pre-sintered, obtain zinc oxide resistance sheet pre- half into
Product, and the pre-sintered maximum temperature is 760~770 DEG C.
7. a kind of zinc oxide resistance sheet as claimed in claim 6, it is characterised in that the pre-sintering is specially：It is described secondary
Sintering：The pre- semi-finished product of zinc oxide resistance sheet are subjected to double sintering, to obtain zinc oxide resistance sheet semi-finished product, and the secondary burning
The maximum temperature of knot is 1050 ± 10 DEG C.
8. a kind of production technology of zinc oxide resistance sheet, it is characterised in that comprise the following steps：
S1. raw material is prepared, and adhesive is added in the raw material of the zinc oxide resistance sheet and water carries out ball milling mixing, to be gone out
Expect 1 μm~2 μm of particle diameter, viscosity is 40~90MPas, and the slurry of 40~65 parts of slurry solid content；
S2. drying-granulating：By the slurry obtained by step S1 by granulating and drying tower with drying-granulating, and through 100 mesh vibratory sieves,
To obtain granulation material of the moisture content as (0.4 ± 0.1) part；
S3. it is dry-pressing formed：Granulation material is pressed into the zinc oxide resistance sheet preform of preset shape, the zinc oxide resistance sheet
Density meets ρ=(3.15 ± 0.05) g/cm3；
S4. sinter：The zinc oxide resistance sheet preform is sintered, obtains zinc oxide resistance sheet semi-finished product；
S5. it is electrode coated：In the electrode coated slurry of upper and lower surface of the zinc oxide resistance sheet semi-finished product, zinc oxide is obtained after firing
Resistor disc.
9. a kind of production technology of zinc oxide resistance sheet as claimed in claim 8, it is characterised in that the sintering step includes
Pre-sintered and double sintering, wherein,
The pre-sintering concretely comprises the following steps：First the zinc oxide resistance sheet preform places kiln, by the temperature of kiln in 16h
400 DEG C continuously are risen to, then, is incubated 4h every time, kiln temperature is raised 100 DEG C every time, until temperature rises to 760~770 DEG C,
Soaking time 12h, then ladder is cooled to 560 DEG C of insulation 4h, then is cooled to 420 DEG C, kiln discharge, naturally cools to normal temperature, with
To the pre- semi-finished product of zinc oxide resistance sheet.
A kind of 10. production technology of zinc oxide resistance sheet as claimed in claim 9, it is characterised in that the double sintering tool
Body step is：The pre- semi-finished product of initial oxidation zinc resistor disc place kiln, and the temperature of kiln is continuously risen into 800 DEG C ± 10 DEG C in 16h,
18h is incubated, then, temperature is risen to 920, is incubated 8h, then temperature is risen to 1050 DEG C ± 10 DEG C, 16~17h of soaking time, so
After be cooled to 870 DEG C insulation 4h, then cool again 760 DEG C, kiln discharge, naturally cool to normal temperature, to obtain obtaining zinc oxide resistance sheet
Semi-finished product.
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| CN109741893A (en) * | 2018-11-28 | 2019-05-10 | 清华大学 | It is resistant to the Zinc-oxide piezoresistor side high-resistance layer preparation process of 4/10 μ s heavy current impact |
| CN111662096A (en) * | 2020-05-13 | 2020-09-15 | 江苏大学 | Sealing method of ceramic capacitor pressure sensor chip |
| CN114994140A (en) * | 2022-05-24 | 2022-09-02 | 哈尔滨工业大学 | Zinc oxide-titanium dioxide sensor for detecting sulfur content and preparation method and application thereof |
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