CN107629466A - A kind of function slurry for chip macromolecule static suppressor - Google Patents
A kind of function slurry for chip macromolecule static suppressor Download PDFInfo
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Abstract
The invention discloses a kind of function slurry for chip macromolecule static suppressor, including following component by weight percentage：30 40 parts of organic carrier, 20 30 parts of conductive material, 10 20 parts of semi-conducting material, 5 10 parts of barium sulfate, 15 parts of glass microballoon, 15 parts of dispersant.The material can prevent that metal from contacting with each other the material electric leakage of initiation, prevents conductive material from aoxidizing in process of production, causes the operating voltage of device to increase, while can also adjust the thickness of surface integument, so as to adjust electrostatic trigger voltage, improves the stability of product.
Description
Technical field
The present invention relates to technical field of composite materials, more particularly to a kind of function for chip macromolecule static suppressor
Slurry and preparation method thereof.
Background technology
Voltage-sensitive ceramic refers to semiconductive ceramic of the resistance value with applied voltage into notable non-linear relation.Thus manufactured pressure
The resistance of quick resistance can be reciprocal between linear high-impedance state and the low resistive state of approximate conducting with the lifting of outer field voltage
Conversion, it is a kind of typical " intelligent " electronic component.Piezo-resistance is generally in parallel with by protection circuit or electronic component, works as circuit
In when thering is the overload to occur, piezo-resistance can automatically will overload bypass so that circuit or element are exempted from along bad.
First, Zinc-oxide piezoresistor
Zinc-oxide piezoresistor is a kind of based on ZnO, adds Multimetal oxide (Bi2O3、MnO2、Co2O3、
Cr2O3、Sb2O3Deng), the polycrystalline ceramic formed with ceramic process sintering, its current-voltage (I-V) characteristic is similar to two-way neat
Receive diode, have very high non-linear.Using ZnO crystal grain as principal crystalline phase, size exists zinc oxide nonlinear resistance slice after burning till
It is several, tens microns, belong to N-type semiconductor；It is very thin grain boundary layer around ZnO crystal grain, about tens nanometers of thickness, grain boundary layer contains
Abundant surface state.Double Schottky barriers are formed in cooling procedure between grain boundary layer and crystal grain, therefore each grain boundary layer is exactly one
Individual small nonlinear resistive element；Because its I-V characteristic is similar to bi-directional zener diode, the resistance under normal working voltage
Value is very high, close to mega-ohms, increases, resistance drastically declines, and in surge voltage impact, resistance only has several Europe with voltage
Several ohm of nurse, even zero point, it is seen that resistance changes with voltage, i.e., with significant nonlinear characteristic.
ZnO voltage-sensitive ceramics are because with high non-linearity, high surge absoption ability, response is fast, inexpensive, manufacture craft is simple
Just the features such as, the most wide piezoresistive material of application is had become at present.ZnO varistor is initially widely used in respectively
In kind high-tension circuit, the infringement of moment overload (such as thunder and lightning) to circuit is prevented.With the high speed development of electronic information technology, low
The sub- antistatic field of piezoelectricity, reliability is high, and the stacked ZnO varistor of miniaturization is widely used.
But with the transmission frequency more and more higher of electronic signal, the leakage of the bulky capacitor and microampere order of stacked piezo-resistance
Electric current has been unable to meet demand.
2nd, macromolecule antistatic (PESD) element
PESD is the macromolecule pressure sensitive that embedded conductor, semiconductor and insulating particle are formed in the polymer.Its resistance
It is in nonlinear change with both end voltage；When the voltage for being applied to its both ends is less than some particular voltage level, PESD is rendered as absolutely
Edge body, resistance is very big, does not influence the normal work of circuit；When the voltage for being applied to both ends is more than some particular voltage level,
PESD is changed into conductor, resistance very little, can with short time heavy-current discharge, therefore can with it is used in parallel by protection circuit.Simultaneously
This PESD electrostatic protection elements have self-reparability, i.e., return to normality again after overvoltage electric discharge, it is not necessary to change, Ke Yiyou
Effect prevents being destroyed by electrostatic impact for electronic product.Because PESD materials are made up of polymer-based, it is impossible to bear height
Temperature, and easily polluted by process；But because high polymer material has higher hydrophobic performance, therefore the device prepared in itself
Affected by environment relatively low, the stability and reliability of device are higher.
Chinese patent 201110103006, Publication No. CN102220109A, disclose a kind of slurry for electrostatic devices
Preparation method for material, comprise the following steps：Glass fluxing technique raw material is prepared, this glass fluxing technique raw material includes calcium isopropoxide, the fourth of boric acid three
Fat, aluminium ethylate, tetraethyl silicate resin；Ethyl cellulose, castor oil and surfactant are added into the terpinol and obtain pine tar
Alcohol carrier；The glass fluxing technique raw material and the pine tar alcohol carrier are mixed and stirred for it after being completely dissolved, are cooled to room temperature
So as to form paste carrier；Cobalt sesquioxide, manganese dioxide, silica, nickel oxide and chrome green are doped to oxidation
In zinc powder；The Zinc oxide particles of the semiconducting and aluminum particle are put into the paste carrier with inorganic non-conductive,
The inorganic non-conductive is Al2O3, SiO2, any one in CaO, MgO or their any mixture.The invention system
Preparation Method, which obtains antistatic zinc oxide material, has strong resistance to electrostatic impact ability, leakage current under normal operating conditions can be down into 1 μ
Below A.But it is not strong to the impact property of functional material to preventing electric arc, reliability and stability are poor.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of for chip macromolecule static suppressor
Function slurry, the reliability and stability of device can be improved.
A kind of function slurry for chip macromolecule static suppressor, including following component by weight percentage：
Organic carrier 30-40 parts, conductive material 20-30 parts, semi-conducting material 10-20 parts, barium sulfate 5-10 parts, glass microballoon 1-5 parts,
Dispersant 1-5 parts.
Preferably, the organic carrier includes following component by weight percentage：Fluorosioloxane rubber or flexible silica gel 20-
40 parts, isophorone 45-60 parts, lauryl alcohol ester 10-15 parts, 2-HEPTANONE 10-15 parts, levelling agent 1-3 parts, surfactant 1-5
Part.
Preferably, the conductive material includes following component by weight percentage：It is metal-powder 10-20 parts, anhydrous
Ethanol 50-80 parts, watery hydrochloric acid 5-10 parts, concentrated ammonia liquor 15-20 parts, tetraethyl orthosilicate 7.5-10 parts, deionized water 20-30 parts,
Wherein the concentration of watery hydrochloric acid be 5% (w%), the concentration of concentrated ammonia liquor be 15-20% (w%).
Preferably, the metal-powder is the one or more in Fe powder, Cu powder, Al powder, Ni powder, the metal-powder
Top layer is covered with SiO2Film, the particle diameter of the metal-powder is 1-4 μm.
Preferably, the semi-conducting material includes following component by weight percentage：ZnO 90-97 parts, Co2O3
0.5-0.7 parts, SiO20.5-1.0 parts, Cr2O30.5-1.0 parts, Sb2O30.5-1.0 parts, MnO20.5-1.0 parts, NiO
0.5-1.0 parts, Y2O30.5-1.0 parts.
Preferably, the semi-conducting material is spherical particles, a diameter of 0.8-1.2 μm of its middle position.
Preferably, the barium sulfate is armorphous nano class B insulation powder stuffing, 1-3 μm of the particle diameter of the glass microballoon.
A kind of preparation method of function slurry for chip macromolecule static suppressor, it is characterised in that method and step
It is as follows：S1：Conductive material, semi-conducting material, barium sulfate, glass microballoon, dispersant are put into progress tank mill in plastic tank, then
325 mesh sieves are crossed by ultrasonic disperse, that is, obtain pre-mixing function powder；S2：By pre-mixing function powder made from S1, addition has airborne
Body, then by three-roll grinder, it is ground to below fineness 5um.
Further, the tank time consuming of the S1 is 45-50h.
In the present invention, the preparation method of organic carrier is as follows：
S1：Isophorone and lauryl alcohol ester are inserted in round-bottomed flask, are well mixed；
S2：The mixed solution obtained in S1 is heated to 60 DEG C in a water bath, then by fluorosioloxane rubber be dispersed into fritter by
Step adds, and uniform stirring 24h, after translucent rubber is completely dissolved, adds levelling agent BYK333 and surfactant
PEG-400, obtain organic carrier.
In the present invention, the preparation method of conductive material is as follows：
S1：Measured according to following ratio：Absolute ethyl alcohol, watery hydrochloric acid, deionized water, metal-powder are inserted in container,
N2Stir process 6-12h in the lower heating water bath of protection, bath temperature is 40 DEG C, removes surface oxide layer；
S2：Concentrated ammonia liquor is added dropwise in S1 container, is added dropwise to complete rear uniform stirring 6-12h, makes the metal ion in solution
After the precipitation of formation is completely dissolved, mass percent 7.5-10% tetraethyl orthosilicate is then added, tetraethyl orthosilicate adds
Enter speed for 1 drop/sec；
S3：The mixture that reaction obtained by S2 is completed, sedimentation or centrifugation remove supernatant, and sediment is dried through high temperature
Afterwards, 300 DEG C of sintering 2h, that is, the conductive material wrapped up in Muffle furnace.
Metal-powder outer layer SiO2The preparation principle of film is as follows：
Reaction equation is as follows by taking Ni as an example：Note：@is the meaning of parcel
Ni@NiO+2HCl→Ni+Ni2++2Cl-+H2O
Remove removing oxide layer；
Metal surface ammonification；
In the present invention, the preparation method of semi-conducting material is as follows：
S1：By ZnO, Co2O3、SiO2、Cr2O3、Sb2O3、MnO、NiO、Y2O3It is put into ball grinder, and it is anhydrous to add 100mL
Ethanol, then ball milling 48 hours in the planetary ball mill that ratio of grinding media to material is 7: 1, rotating speed 350rpm, gained powder dry through 80 DEG C
ZnO doping powder is obtained after dry 6h；
S2：After the ZnO doping powder obtained in S1 is dried, the adhesive for adding powder weight 1-5% is mixed into bulk, so
After pressurize 30MPa, 80 mesh sieves are crossed after about 12h, dry 2h at 150 DEG C after sieving, are subsequently placed in 1200 DEG C of calcination 4 in whirl-sintering furnace
Hour obtains the powder of pre-burning；
S3：The powder of the pre-burning obtained in S2 is put into the absolute ethyl alcohol that 80-100mL is added in ball grinder, then in ball
Material is than being 2: 1, ball milling 0.5h in rotating speed 350rpm planetary ball mill, and it is 1.0 μm to obtain obtaining meso-position radius after drying
Spherical semiconductor material oxidation zinc particle.
Compared with the prior art, the present invention has the beneficial effect that：
1st, organic carrier adhesive of the invention is fluorosioloxane rubber, has certain elasticity after solidification, can effectively prevent
Only impact of the electric arc to functional material；Stability is higher, itself has higher insulating properties, and energy security function slurry is in height
It will not be leaked electricity in pressure impact process caused by carbonization.
2nd, semi-conducting material zinc oxide of the present invention is spherical that can improve its decentralization in the slurry, and its surface is present
Complete crystal boundary, it is filled in function slurry, its resistance to electrostatic impact ability can be greatly improved, and reduce normal operating conditions
Clamped voltage and leakage current.
3rd, conductive particle of the present invention takes packing technology to handle, and to prevent that surface insulation layer is uneven, therefore is wrapping up
Before, the oxide layer on surface is fallen using acid treatment, adsorbed by ammoniacal liquor, TEOS hydrolysis, it is 20- to make metal surface clad
50nm SiO2Layer, the integument belong to mesoporous material, and inside has nano-pore, can pass through electronics or ion, moreover it is possible to prevent
Metal contact with each other initiation material electric leakage, prevent conductive material from aoxidizing in process of production, cause the operating voltage of device to increase
Height, while the thickness of surface integument can also be adjusted, so as to adjust electrostatic trigger voltage.
4th, the present invention use spherical glass beads, has preferably dispersiveness, and itself is with compared with high-insulativity, higher hard
Degree, pricked in slurry roller and play lubrication in slurry printing process, prevent the parcel damage layer and metal sheeting of metal material
Trigger electric leakage, so as to improve the reliability and stability of device.
5th, the addition of nano-barium sulfate powder, barium sulfate powder have the property of higher insulating properties and acid-alkali-corrosive-resisting
Can, because fluorosioloxane rubber forms network structure after function slurry curing, easily it is squeezed and deforms upon, triggers electrical property not
It is good.The filling of nano barium sulfate can improve the stability of function slurry and anti-extrusion performance, and the conduct when electrostatic impacts
To the cushion of metal material, so as to reduce the trigger voltage of device and improve device stability.
Brief description of the drawings
Fig. 1 is the electron microscopic picture for the metal-powder that before processing is wrapped up in embodiment 1；
Fig. 2 is the electron microscopic picture of the metal-powder after parcel processing in embodiment 1；
Fig. 3 is the electron microscopic picture of spherical semiconductor ZnO powders in embodiment 1；
Fig. 4 is the electron microscopic picture after function slurry curing in embodiment 1.
In figure：Metal powder, 3- integuments SiO after the non-coated metal powder of 1-, 2- parcels2, the spherical zinc oxide of 4-, 5- surfaces
Crystal boundary, the space in 6- function slurries, the fluorosioloxane rubber in 7- function slurries, semiconductor ZnO, 9- function in 8- function slurries
The barium sulphate nano powder in coated metal powder, 10- function slurries in slurry.
Embodiment
The present invention is made with reference to specific embodiment further to explain.
Embodiment 1
1st, the preparation of organic carrier
Organic carrier includes following component by weight percentage：20 parts of fluorosioloxane rubber, 45 parts of isophorone, lauryl alcohol
10 parts of ester, 10 parts of 2-HEPTANONE, 1 part of levelling agent, 1 part of surfactant.
The preparation method of organic carrier, method and step are as follows：
S1：Isophorone, lauryl alcohol ester, 2-HEPTANONE are inserted in round-bottomed flask, are well mixed；S2：By what is obtained in S1
Mixed solution is heated to 60 DEG C in a water bath, and fluorosioloxane rubber then is dispersed into fritter is gradually added, uniform stirring 24h, treats half
After transparence rubber is completely dissolved, levelling agent BYK333 and Surfactant PEG -400 are added, obtain organic carrier.
2nd, the preparation of conductive material
Conductive material includes following component by weight percentage：10 parts of metal-powder, 50 parts of absolute ethyl alcohol, watery hydrochloric acid
5 parts, 15 parts of concentrated ammonia liquor, 7.5 parts of tetraethyl orthosilicate, 20 parts of deionized water.
Wherein, metal-powder is Fe powder, and the particle diameter of metal-powder is 1 μm；The concentration of watery hydrochloric acid is 5% (w%)；Concentrated ammonia liquor
Concentration be 15% (w%).
The preparation method of conductive material, method and step are as follows：
S1：Measured according to following ratio：Absolute ethyl alcohol, watery hydrochloric acid, deionized water, metal-powder are inserted in container,
N2Stir process 6h in the lower heating water bath of protection, bath temperature is 40 DEG C, removes surface oxide layer；
S2：Concentrated ammonia liquor is added dropwise in S1 container, is added dropwise to complete rear uniform stirring 6h, forms the metal ion in solution
Precipitation be completely dissolved after, then add mass percent 7.5% tetraethyl orthosilicate, tetraethyl orthosilicate add speed be
1 drop/sec；
S3：The mixture that reaction obtained by S2 is completed, sedimentation or centrifugation remove supernatant, and sediment is dried through high temperature
Afterwards, 300 DEG C of sintering 2h, that is, the conductive material wrapped up in Muffle furnace.
3rd, the preparation of semi-conducting material
Semi-conducting material includes following component by weight percentage：90 parts of ZnO, Co2O30.5 part, SiO2 0.5
Part, Cr2O30.5 part, Sb2O30.5 part, MnO20.5 part, 0.5 part of NiO, Y2O30.5 part.
The preparation method of semi-conducting material, method and step are as follows：
S1：By ZnO, Co2O3、SiO2、Cr2O3、Sb2O3、MnO、NiO、Y2O3It is put into ball grinder, and it is anhydrous to add 100mL
Ethanol, then ball milling 48 hours in the planetary ball mill that ratio of grinding media to material is 7: 1, rotating speed 350rpm, gained powder dry through 80 DEG C
ZnO doping powder is obtained after dry 6h；
S2：After the ZnO doping powder obtained in S1 is dried, the adhesive for adding powder weight 1% is mixed into bulk, then
Pressurize 30MPa, crosses 80 mesh sieves after about 12h, dries 2h at 150 DEG C after sieving, and it is small to be subsequently placed in 1200 DEG C of calcination 4 in whirl-sintering furnace
When obtain pre-burning powder；
S3：The powder of the pre-burning obtained in S2 is put into the absolute ethyl alcohol that 80mL is added in ball grinder, then in ratio of grinding media to material
For 2: 1, ball milling 0.5h in rotating speed 350rpm planetary ball mill, it is 1.0 μm spherical to obtain obtaining meso-position radius after drying
Semi-conducting material Zinc oxide particles.
4th, the preparation of function slurry
A kind of function slurry for chip macromolecule static suppressor, including following component by weight percentage：
30 parts of organic carrier, 20 parts of conductive material, 10 parts of semi-conducting material, 5 parts of barium sulfate, 1 part of glass microballoon, 1 part of dispersant.
A kind of preparation method of function slurry for chip macromolecule static suppressor, method and step are as follows：
S1：Conductive material, semi-conducting material, barium sulfate, glass microballoon, dispersant are put into progress tank mill in plastic tank,
Tank time consuming is 45h, then crosses 325 mesh sieves by ultrasonic disperse, that is, obtains pre-mixing function powder；S2：By premix made from S1
Function powder, organic carrier is added, then by three-roll grinder, is ground to below fineness 5um.
Embodiment 2
1st, the preparation of organic carrier
Organic carrier includes following component by weight percentage：Fluorosioloxane rubber or 40 parts of flexible silica gel, isophorone
60 parts, 15 parts of lauryl alcohol ester, 15 parts of 2-HEPTANONE, 3 parts of levelling agent, 5 parts of surfactant.
The preparation method of organic carrier is the same as embodiment 1.
2nd, the preparation of conductive material
Conductive material includes following component by weight percentage：20 parts of metal-powder, 80 parts of absolute ethyl alcohol, watery hydrochloric acid
10 parts, 20 parts of concentrated ammonia liquor, 10 parts of tetraethyl orthosilicate, 30 parts of deionized water.
Wherein, metal-powder is Cu powder, and the particle diameter of metal-powder is 4 μm；The concentration of watery hydrochloric acid is 5% (w%)；Concentrated ammonia liquor
Concentration be 20% (w%).
The preparation method of conductive material, method and step are as follows：
S1：Measured according to following ratio：Absolute ethyl alcohol, watery hydrochloric acid, deionized water, metal-powder are inserted in container,
N2Stir process 12h in the lower heating water bath of protection, bath temperature is 40 DEG C, removes surface oxide layer；
S2：Concentrated ammonia liquor is added dropwise in S1 container, is added dropwise to complete rear uniform stirring 12h, makes the metal ion shape in solution
Into precipitation be completely dissolved after, then add mass percent 10% tetraethyl orthosilicate, tetraethyl orthosilicate add speed
For 1 drop/sec；
S3：The mixture that reaction obtained by S2 is completed, sedimentation or centrifugation remove supernatant, and sediment is dried through high temperature
Afterwards, 300 DEG C of sintering 2h, that is, the conductive material wrapped up in Muffle furnace.
3rd, the preparation of semi-conducting material
Semi-conducting material includes following component by weight percentage：97 parts of ZnO, Co2O30.7 part, SiO2 1.0
Part, Cr2O31.0 parts, Sb2O31.0 parts, MnO21.0 parts, 1.0 parts of NiO, Y2O31.0 part.
The preparation method of semi-conducting material, method and step are as follows：
S1：By ZnO, Co2O3、SiO2、Cr2O3、Sb2O3、MnO、NiO、Y2O3It is put into ball grinder, and it is anhydrous to add 100mL
Ethanol, then ball milling 48 hours in the planetary ball mill that ratio of grinding media to material is 7: 1, rotating speed 350rpm, gained powder dry through 80 DEG C
ZnO doping powder is obtained after dry 6h；
S2：After the ZnO doping powder obtained in S1 is dried, the adhesive for adding powder weight 5% is mixed into bulk, then
Pressurize 30MPa, crosses 80 mesh sieves after about 12h, dries 2h at 150 DEG C after sieving, and it is small to be subsequently placed in 1200 DEG C of calcination 4 in whirl-sintering furnace
When obtain pre-burning powder；
S3：The powder of the pre-burning obtained in S2 is put into the absolute ethyl alcohol that 100mL is added in ball grinder, then in ratio of grinding media to material
For 2: 1, ball milling 0.5h in rotating speed 350rpm planetary ball mill, it is 1.0 μm spherical to obtain obtaining meso-position radius after drying
Semi-conducting material Zinc oxide particles.
5th, the preparation of function slurry
A kind of function slurry for chip macromolecule static suppressor, including following component by weight percentage：
40 parts of organic carrier, 30 parts of conductive material, 20 parts of semi-conducting material, 10 parts of barium sulfate, 5 parts of glass microballoon, 5 parts of dispersant.
A kind of preparation method of function slurry for chip macromolecule static suppressor, method and step are as follows：
S1：Conductive material, semi-conducting material, barium sulfate, glass microballoon, dispersant are put into progress tank mill in plastic tank,
Tank time consuming is 50h, then crosses 325 mesh sieves by ultrasonic disperse, that is, obtains pre-mixing function powder；S2：By premix made from S1
Function powder, organic carrier is added, then by three-roll grinder, is ground to below fineness 5um.
Embodiment 3
1st, the preparation of organic carrier
Organic carrier includes following component by weight percentage：Fluorosioloxane rubber or 30 parts of flexible silica gel, isophorone
50 parts, 12 parts of lauryl alcohol ester, 13 parts of 2-HEPTANONE, 2 parts of levelling agent, 3 parts of surfactant.
The preparation method of organic carrier is the same as embodiment 1.
2nd, the preparation of conductive material
Conductive material includes following component by weight percentage：15 parts of metal-powder, 65 parts of absolute ethyl alcohol, watery hydrochloric acid
8 parts, 16 parts of concentrated ammonia liquor, 8 parts of tetraethyl orthosilicate, 25 parts of deionized water.
Wherein, metal-powder is Al powder, and the particle diameter of metal-powder is 2 μm；The concentration of watery hydrochloric acid is 5% (w%)；Concentrated ammonia liquor
Concentration be 17% (w%).
The preparation method of conductive material, method and step are as follows：
S1：Measured according to following ratio：Absolute ethyl alcohol, watery hydrochloric acid, deionized water, metal-powder are inserted in container,
N2Stir process 10h in the lower heating water bath of protection, bath temperature is 40 DEG C, removes surface oxide layer；
S2：Concentrated ammonia liquor is added dropwise in S1 container, is added dropwise to complete rear uniform stirring 8h, forms the metal ion in solution
Precipitation be completely dissolved after, then add mass percent 8.5% tetraethyl orthosilicate, tetraethyl orthosilicate add speed be
1 drop/sec；
S3：The mixture that reaction obtained by S2 is completed, sedimentation or centrifugation remove supernatant, and sediment is dried through high temperature
Afterwards, 300 DEG C of sintering 2h, that is, the conductive material wrapped up in Muffle furnace.
3rd, the preparation of semi-conducting material
Semi-conducting material includes following component by weight percentage：95 parts of ZnO, Co2O30.6 part, SiO2 0.8
Part, Cr2O30.7 part, Sb2O30.6 part, MnO20.6 part, 0.7 part of NiO, Y2O30.7 part.
The preparation method of semi-conducting material, method and step are as follows：
S1：By ZnO, Co2O3、SiO2、Cr2O3、Sb2O3、MnO、NiO、Y2O3It is put into ball grinder, and it is anhydrous to add 100mL
Ethanol, then ball milling 48 hours in the planetary ball mill that ratio of grinding media to material is 7: 1, rotating speed 350rpm, gained powder dry through 80 DEG C
ZnO doping powder is obtained after dry 6h；
S2：After the ZnO doping powder obtained in S1 is dried, the adhesive for adding powder weight 3% is mixed into bulk, then
Pressurize 30MPa, crosses 80 mesh sieves after about 12h, dries 2h at 150 DEG C after sieving, and it is small to be subsequently placed in 1200 DEG C of calcination 4 in whirl-sintering furnace
When obtain pre-burning powder；
S3：The powder of the pre-burning obtained in S2 is put into the absolute ethyl alcohol that 90mL is added in ball grinder, then in ratio of grinding media to material
For 2: 1, ball milling 0.5h in rotating speed 350rpm planetary ball mill, it is 1.0 μm spherical to obtain obtaining meso-position radius after drying
Semi-conducting material Zinc oxide particles.
6th, the preparation of function slurry
A kind of function slurry for chip macromolecule static suppressor, including following component by weight percentage：
35 parts of organic carrier, 25 parts of conductive material, 15 parts of semi-conducting material, 8 parts of barium sulfate, 3 parts of glass microballoon, 3 parts of dispersant.
A kind of preparation method of function slurry for chip macromolecule static suppressor, method and step are as follows：
S1：Conductive material, semi-conducting material, barium sulfate, glass microballoon, dispersant are put into progress tank mill in plastic tank,
Tank time consuming is 48h, then crosses 325 mesh sieves by ultrasonic disperse, that is, obtains pre-mixing function powder；S2：By premix made from S1
Function powder, organic carrier is added, then by three-roll grinder, is ground to below fineness 5um.
Embodiment 4
1st, the preparation of organic carrier
Organic carrier includes following component by weight percentage：Fluorosioloxane rubber or 25 parts of flexible silica gel, isophorone
55 parts, 11 parts of lauryl alcohol ester, 12 parts of 2-HEPTANONE, 2 parts of levelling agent, 2 parts of surfactant.
The preparation method of organic carrier is the same as embodiment 1.
2nd, the preparation of conductive material
Conductive material includes following component by weight percentage：13 parts of metal-powder, 60 parts of absolute ethyl alcohol, watery hydrochloric acid
6 parts, 18 parts of concentrated ammonia liquor, 9 parts of tetraethyl orthosilicate, 23 parts of deionized water.
Wherein, metal-powder is Ni powder, and the particle diameter of metal-powder is 3 μm；The concentration of watery hydrochloric acid is 5% (w%)；Concentrated ammonia liquor
Concentration be 16% (w%).
The preparation method of conductive material, method and step are as follows：
S1：Measured according to following ratio：Absolute ethyl alcohol, watery hydrochloric acid, deionized water, metal-powder are inserted in container,
N2Stir process 8h in the lower heating water bath of protection, bath temperature is 40 DEG C, removes surface oxide layer；
S2：Concentrated ammonia liquor is added dropwise in S1 container, is added dropwise to complete rear uniform stirring 11h, makes the metal ion shape in solution
Into precipitation be completely dissolved after, then add mass percent 9% tetraethyl orthosilicate, tetraethyl orthosilicate add speed be
1 drop/sec；
S3：The mixture that reaction obtained by S2 is completed, sedimentation or centrifugation remove supernatant, and sediment is dried through high temperature
Afterwards, 300 DEG C of sintering 2h, that is, the conductive material wrapped up in Muffle furnace.
3rd, the preparation of semi-conducting material
Semi-conducting material includes following component by weight percentage：93 parts of ZnO, Co2O30.6 part, SiO2 0.9
Part, Cr2O30.7 part, Sb2O30.8 part, MnO20.7 part, 0.8 part of NiO, Y2O30.9 part.
The preparation method of semi-conducting material, method and step are as follows：
S1：By ZnO, Co2O3、SiO2、Cr2O3、Sb2O3、MnO、NiO、Y2O3It is put into ball grinder, and it is anhydrous to add 100mL
Ethanol, then ball milling 48 hours in the planetary ball mill that ratio of grinding media to material is 7: 1, rotating speed 350rpm, gained powder dry through 80 DEG C
ZnO doping powder is obtained after dry 6h；
S2：After the ZnO doping powder obtained in S1 is dried, the adhesive for adding powder weight 3% is mixed into bulk, then
Pressurize 30MPa, crosses 80 mesh sieves after about 12h, dries 2h at 150 DEG C after sieving, and it is small to be subsequently placed in 1200 DEG C of calcination 4 in whirl-sintering furnace
When obtain pre-burning powder；
S3：The powder of the pre-burning obtained in S2 is put into the absolute ethyl alcohol that 80-100mL is added in ball grinder, then in ball
Material is than being 2: 1, ball milling 0.5h in rotating speed 350rpm planetary ball mill, and it is 1.0 μm to obtain obtaining meso-position radius after drying
Spherical semiconductor material oxidation zinc particle.
7th, the preparation of function slurry
A kind of function slurry for chip macromolecule static suppressor, including following component by weight percentage：
33 parts of organic carrier, 28 parts of conductive material, 17 parts of semi-conducting material, 6 parts of barium sulfate, 2 parts of glass microballoon, 4 parts of dispersant.
A kind of preparation method of function slurry for chip macromolecule static suppressor, method and step are as follows：
S1：Conductive material, semi-conducting material, barium sulfate, glass microballoon, dispersant are put into progress tank mill in plastic tank,
Tank time consuming is 49h, then crosses 325 mesh sieves by ultrasonic disperse, that is, obtains pre-mixing function powder；S2：By premix made from S1
Function powder, organic carrier is added, then by three-roll grinder, is ground to below fineness 5um.
Embodiment 5
1st, the preparation of organic carrier
Organic carrier includes following component by weight percentage：Fluorosioloxane rubber or 35 parts of flexible silica gel, isophorone
50 parts, 14 parts of lauryl alcohol ester, 14 parts of 2-HEPTANONE, 2 parts of levelling agent, 2 parts of surfactant.
The preparation method of organic carrier is the same as embodiment 1.
2nd, the preparation of conductive material
Conductive material includes following component by weight percentage：18 parts of metal-powder, 75 parts of absolute ethyl alcohol, watery hydrochloric acid
9 parts, 19 parts of concentrated ammonia liquor, 9.5 parts of tetraethyl orthosilicate, 27 parts of deionized water.
Wherein, metal-powder is that Fe powder and Cu powder in mass ratio 1: 1 are prepared, and the particle diameter of metal-powder is 2 μm；Watery hydrochloric acid
Concentration is 5% (w%)；The concentration of concentrated ammonia liquor is 19% (w%).
The preparation method of conductive material, method and step are as follows：
S1：Measured according to following ratio：Absolute ethyl alcohol, watery hydrochloric acid, deionized water, metal-powder are inserted in container,
N2Stir process 8h in the lower heating water bath of protection, bath temperature is 40 DEG C, removes surface oxide layer；
S2：Concentrated ammonia liquor is added dropwise in S1 container, is added dropwise to complete rear uniform stirring 7h, forms the metal ion in solution
Precipitation be completely dissolved after, then add mass percent 7.5-10% tetraethyl orthosilicate, tetraethyl orthosilicate adds speed
Spend for 1 drop/sec；
S3：The mixture that reaction obtained by S2 is completed, sedimentation or centrifugation remove supernatant, and sediment is dried through high temperature
Afterwards, 300 DEG C of sintering 2h, that is, the conductive material wrapped up in Muffle furnace.
3rd, the preparation of semi-conducting material
Semi-conducting material includes following component by weight percentage：96 parts of ZnO, Co2O30.6 part, SiO2 0.6
Part, Cr2O30.6 part, Sb2O30.9 part, MnO20.6 part, 0.6 part of NiO, Y2O30.8 part.
The preparation method of semi-conducting material, method and step are as follows：
S1：By ZnO, Co2O3、SiO2、Cr2O3、Sb2O3、MnO、NiO、Y2O3It is put into ball grinder, and it is anhydrous to add 100mL
Ethanol, then ball milling 48 hours in the planetary ball mill that ratio of grinding media to material is 7: 1, rotating speed 350rpm, gained powder dry through 80 DEG C
ZnO doping powder is obtained after dry 6h；
S2：After the ZnO doping powder obtained in S1 is dried, the adhesive for adding powder weight 1-5% is mixed into bulk, so
After pressurize 30MPa, 80 mesh sieves are crossed after about 12h, dry 2h at 150 DEG C after sieving, are subsequently placed in 1200 DEG C of calcination 4 in whirl-sintering furnace
Hour obtains the powder of pre-burning；
S3：The powder of the pre-burning obtained in S2 is put into the absolute ethyl alcohol that 95mL is added in ball grinder, then in ratio of grinding media to material
For 2: 1, ball milling 0.5h in rotating speed 350rpm planetary ball mill, it is 1.0 μm spherical to obtain obtaining meso-position radius after drying
Semi-conducting material Zinc oxide particles.
8th, the preparation of function slurry
A kind of function slurry for chip macromolecule static suppressor, including following component by weight percentage：
38 parts of organic carrier, 22 parts of conductive material, 13 parts of semi-conducting material, 7 parts of barium sulfate, 3 parts of glass microballoon, 2 parts of dispersant.
A kind of preparation method of function slurry for chip macromolecule static suppressor, method and step are as follows：
S1：Conductive material, semi-conducting material, barium sulfate, glass microballoon, dispersant are put into progress tank mill in plastic tank,
Tank time consuming is 45-50h, then crosses 325 mesh sieves by ultrasonic disperse, that is, obtains pre-mixing function powder；S2：Will be pre- made from S1
Mixed function powder, adds organic carrier, then by three-roll grinder, is ground to below fineness 5um.
Material property detects
1st, detection method：
(1) impact resistance：The slurry is placed in macromolecule static suppressor by typography, tests electrical property, it is resistance to
Impulsive force test is main to be evaluated as static gun ± 8KV impacts, and interval time 1S, number of blows is 1000 times, appearance of device without
Damage, electrical property are unchanged.
(2) stability test is mainly evaluated as anti-pulse ability：The slurry is placed in macromolecule electrostatic by typography
In suppressor, test the ability of the anti-pulse of device by onoff, voltage 12V, break-make at intervals of 5 seconds and logical 5s disconnected 5s,
Testing time is 1000 times, outward appearance and drain conditions is detected after the completion of test, appearance of device is without damage, no electric leakage IL＜ 0.1uA.
(3) performance of high-temp resisting high-humidity resisting (double 85, which are powered, tests)：The slurry is placed in macromolecule electrostatic by typography
In suppressor, completed device is prepared, (test quantity is 200PCS) is placed in test board by Reflow Soldering, leads to 12V voltages, puts
It it is 85 DEG C, in the humidity cabinet of humidity 85% in temperature, the testing time is 1000 hours, total electrical leakage quantity IL＜ 10uA.
(4) high/low temperature circulation experiment：The slurry is placed in macromolecule static suppressor by typography, prepared
Whole device, (test quantity is 200PCS) is placed in test board by Reflow Soldering and is positioned over high/low-temperature impact case, -40 DEG C of low temperature,
85 DEG C of high temperature, circulation time are 1 hour, soaking time 30min, and cycle-index is 20 times, and appearance of device is without damage, no electric leakage
IL＜ 0.1uA.
2nd, testing result：It is shown in Table 1.
The performance test results of table 1
Control group is commercially available macromolecule static suppressor.
3rd, conclusion
The organic carrier of fluorosioloxane rubber system, there is higher insulating properties and certain elasticity after fluorosioloxane rubber solidification, Gu
The electric leakage of material initiation can also be reduced while fixed various materials, while when electrostatic impacts, high energy is reduced by elastic deformation
The impact to material is measured, improves the stability and high reliability of functional material.
Because zinc oxide pressure-sensitive material has the leakage current of microampere order in normal operation, and in electrostatic impact mistake
Afterwards, its leakage current has the trend being stepped up.The present invention is taken in spherical zinc oxide, the complete crystal boundary in surface, can be significantly
Raising its resistance to electrostatic impact ability.The doping of yittrium oxide can reduce the voltage tonsure of pressure sensitive while reduce the leakage of material
Electrical property.
And the purposes of metal powder is for adjusting its electrostatic trigger voltage, but the addition of metal powder can trigger function material
There are a large amount of electric leakages during electrostatic impact in material, and the present invention reduces electrostatic trigger voltage using the conductive material after parcel
The electric leakage that avoids simultaneously, so as to by near below the 1.0uA of the leakage current of normal operating conditions.
Using spherical glass beads, there is preferably dispersiveness, itself has compared with high-insulativity, higher hardness, in slurry
Roller is pricked and plays lubrication in slurry printing process, and the parcel damage layer and metal sheeting for preventing metal material trigger electric leakage,
So as to improve the reliability and stability of device
Barium sulfate powder has the performance of higher insulating properties and acid-alkali-corrosive-resisting, because fluorosioloxane rubber is in function slurry
Network structure is formed after solidification, is easily squeezed and deforms upon, triggers electrical property bad.The filling of nano barium sulfate can carry
The stability and anti-extrusion performance of high function slurry, and when electrostatic impacts as the cushion to metal material, so as to drop
The trigger voltage and raising device stability of low device.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (10)
1. a kind of function slurry for chip macromolecule static suppressor, it is characterised in that including by weight percentage
Following component：Organic carrier 30-40 parts, conductive material 20-30 parts, semi-conducting material 10-20 parts, barium sulfate 5-10 parts, glass
Microballon 1-5 parts, dispersant 1-5 parts.
2. a kind of function slurry for chip macromolecule static suppressor according to claim 1, it is characterised in that described
Organic carrier includes following component by weight percentage：Fluorosioloxane rubber or flexible silica gel 20-40 parts, isophorone 45-60
Part, lauryl alcohol ester 10-15 parts, 2-HEPTANONE 10-15 parts, levelling agent 1-3 parts, surfactant 1-5 parts.
A kind of 3. function slurry for chip macromolecule static suppressor according to claim 1, it is characterised in that institute
Stating conductive material includes following component by weight percentage：Metal-powder 10-20 parts, absolute ethyl alcohol 50-80 parts, watery hydrochloric acid
5-10 parts, concentrated ammonia liquor 15-20 parts, tetraethyl orthosilicate 7.5-10 parts, deionized water 20-30 parts.
A kind of 4. function slurry for chip macromolecule static suppressor according to claim 3, it is characterised in that institute
Metal-powder is stated as the one or more in Fe powder, Cu powder, Al powder, Ni powder, the top layer of the metal-powder is covered with SiO2Film, institute
The particle diameter for stating metal-powder is 1-4 μm.
A kind of 5. function slurry for chip macromolecule static suppressor according to claim 1, it is characterised in that institute
Stating semi-conducting material includes following component by weight percentage：ZnO 90-97 parts, Co2O30.5-0.7 parts, SiO2 0.5-
1.0 parts, Cr2O30.5-1.0 parts, Sb2O30.5-1.0 parts, MnO20.5-1.0 parts, NiO 0.5-1.0 parts, Y2O3 0.5-1.0
Part.
A kind of 6. function slurry for chip macromolecule static suppressor according to claim 5, it is characterised in that institute
It is spherical particles to state semi-conducting material, a diameter of 0.8-1.2 μm of its middle position.
A kind of 7. function slurry for chip macromolecule static suppressor according to claim 1, it is characterised in that institute
It is armorphous nano class B insulation powder stuffing to state barium sulfate, 1-3 μm of the particle diameter of the glass microballoon.
8. a kind of preparation method of function slurry for chip macromolecule static suppressor according to claim 1, its
It is characterised by, method and step is as follows：S1：Conductive material, semi-conducting material, barium sulfate, glass microballoon, dispersant are put into plastics
Tank mill is carried out in tank, 325 mesh sieves are then crossed by ultrasonic disperse, that is, obtain pre-mixing function powder；S2：Work(will be premixed made from S1
Energy powder, adds organic carrier, then by three-roll grinder, is ground to below fineness 5um.
9. a kind of preparation method of function slurry for chip macromolecule static suppressor according to claim 8, its
It is characterised by, the tank time consuming of the S1 is 45-50h.
10. function slurry made from the component described in claim any one of 1-7.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220109A (en) * | 2011-04-25 | 2011-10-19 | 苏州晶讯科技股份有限公司 | Preparation method of sizing applied to electrostatic devices |
| CN104464993A (en) * | 2013-09-12 | 2015-03-25 | 中国振华集团云科电子有限公司 | Method for preparing static-suppressor functional slurry cured at low temperature |
| CN104464992A (en) * | 2013-09-12 | 2015-03-25 | 中国振华集团云科电子有限公司 | Method for preparing functional slurry of chip-type static suppressor |
| CN104650808A (en) * | 2015-02-11 | 2015-05-27 | 苏州晶讯科技股份有限公司 | Slurry for anti-static device |
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- 2017-09-20 CN CN201710851561.6A patent/CN107629466A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220109A (en) * | 2011-04-25 | 2011-10-19 | 苏州晶讯科技股份有限公司 | Preparation method of sizing applied to electrostatic devices |
| CN104464993A (en) * | 2013-09-12 | 2015-03-25 | 中国振华集团云科电子有限公司 | Method for preparing static-suppressor functional slurry cured at low temperature |
| CN104464992A (en) * | 2013-09-12 | 2015-03-25 | 中国振华集团云科电子有限公司 | Method for preparing functional slurry of chip-type static suppressor |
| CN104650808A (en) * | 2015-02-11 | 2015-05-27 | 苏州晶讯科技股份有限公司 | Slurry for anti-static device |
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