CN102220109A - Preparation method of sizing applied to electrostatic devices - Google Patents
Preparation method of sizing applied to electrostatic devices Download PDFInfo
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- CN102220109A CN102220109A CN2011101030068A CN201110103006A CN102220109A CN 102220109 A CN102220109 A CN 102220109A CN 2011101030068 A CN2011101030068 A CN 2011101030068A CN 201110103006 A CN201110103006 A CN 201110103006A CN 102220109 A CN102220109 A CN 102220109A
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- terpineol
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Abstract
The invention discloses a preparation method of sizing applied to electrostatic devices, which comprises the following steps of: preparing a glass-coated raw material comprising isopropanol calcium, tri-n-butyl borate, aluminium ethylate and tetraethyl orthosilicate, adding ethyl cellulose, caster oil and surfactant into terpineol to obtain a terpineol carrier; mixing the glass-coated raw material and the terpineol carrier and stirring until completely dissolving, and cooling to the room temperature to form a pasty carrier; doping cobaltic oxide, manganese dioxide, silicon dioxide, nickel oxide and chromic oxide into zinc oxide powder; and putting semi-conductive zinc oxide particles, aluminium powder particles and an inorganic non-conductive phase into the pasty carrier, wherein the inorganic non-conductive phase is one of or a combination of AI2O3, SiO2, CaO and MgO. The static preventing zinc oxide material obtained by using the preparation method has the strong capability of static shock resistance and is capable of reducing the leakage current in a normal state to be below 1muA.
Description
Technical field
The present invention relates to a kind of antistatic material, be specifically related to a kind of slurry preparation method that is used for electrostatic devices.
Background technology
Voltage-sensitive ceramic is meant that resistance value becomes the semiconductive ceramic of remarkable nonlinear relationship with impressed voltage.The resistance of the voltage dependent resistor of making thus can back and forth be told conversion between the low resistive state of online form height resistance state and approximate conducting along with the lifting of outer field voltage, is a kind of typical case " intelligent " electronic component.Voltage dependent resistor is in parallel with protected circuit or electronic component usually, and when having overload to occur in the circuit, voltage dependent resistor can will be transshipped bypass automatically, thereby circuit or element are exempted from along bad.
Zinc-oxide piezoresistor is a kind of based on ZnO, adds multiple metal oxide (Bi2O3, MnO2, Co2O3, Cr2O3, Sb2O3 etc.), with the polycrystalline ceramic that the ceramic process sintering forms, its current-voltage (I-V) property class is like bi-directional zener diode, has very high non-linear.Zinc oxide nonlinear resistance slice after burning till is a principal crystalline phase with ZnO crystal grain, and size belongs to N-type semiconductor several ~ tens micron; Around the ZnO crystal grain is very thin grain boundary layer, about tens nanometers of thickness, and grain boundary layer contains abundant surface state.Grain boundary layer and intergranule form two Schottky barriers in the process of cooling, therefore each grain boundary layer is exactly a small nonlinear resistive element, and its I-V property class is similar to bi-directional zener diode, and resistance value is very high under normal working voltage, near mega-ohms, along with voltage ground strengthens, resistance sharply descends, when surge voltage is impacted, resistance has only several ohm, or even several ohm of zero points, visible resistance changes with voltage, promptly has significant nonlinear characteristic.
The ZnO voltage-sensitive ceramic because have high non-linearity, high surge receptivity, characteristics, the present the widest piezoresistive material of range of application that become such as response is fast, low-cost, manufacture craft is easy.ZnO varistor is widely used in the various high-tension circuits at first, prevents the infringement of moment overload (as thunder and lightning) to circuit.Along with the high speed development of electronic information technology, in Low-voltage Electronic anti-electrostatic field, the reliability height, the stacked ZnO varistor of miniaturization is widely used.
But along with the transmission frequency of electronic signal is more and more higher, the big electric capacity of stacked voltage dependent resistor and the leakage current of microampere order can not satisfy the demands.
2, polymer anti-electrostatic (PESD) element
PESD is the polymer pressure sensitive that embedded conductor, semi-conductor and insulating particle constitute in polymkeric substance.Its resistance is nonlinearities change with both end voltage.That is to say that when the voltage that is applied to its two ends during less than certain specific voltage value, PESD is rendered as isolator, resistance is very big, does not influence the works better of circuit; When the voltage that is applied to two ends during greater than certain specific voltage value, PESD changes conductor into, and resistance is very little, can the short period of time heavy-current discharge, and therefore can use in parallel with protected circuit.Simultaneously this PESD electrostatic protection element has self-reparability, i.e. return to normality again after the superpotential discharge, needn't change, and can effectively stop being subjected to electrostatic impact of electronic product and destroyed,
Because the PESD material is made up of polymer-based, can not bear high temperature, and be subject to the pollution of the course of processing.Therefore, the tooling cost of PESD element is comparatively expensive, is difficult to realize limited the popularization of product widely as the low-cost scale operation of Zinc-oxide piezoresistor.
Summary of the invention
The object of the invention provides a kind of slurry preparation method that is used for electrostatic devices, and this slurry preparation method obtains the anti-electrostatic zinc oxide material and has strong anti-electrostatic impact ability, leakage current under the normal operating conditions can be reduced to below the 1 μ A.
For achieving the above object, the technical solution used in the present invention is:
A kind of slurry preparation method that is used for electrostatic devices may further comprise the steps:
Step 1, preparation glass coat raw material, and this glass coats the prescription of raw material and mainly is made up of the material of following quality percentage composition:
Calcium isopropoxide (((CH
3)
2CHO)
2Ca), powder, 12%～18%,
Boric acid tri butyl ester (B
2O
3: B (CH
3(CH
2)
3O)
3), powder, 24%～34%,
Aluminum ethylate (Al
2O
3: (CH
3CH
2O)
3Al), powder, 20%～28%,
Tetraethyl silicate resin (SiO
2: Si (OCH
2CH
3)
4), liquid, 27%～37%;
Step 2, Terpineol 350 is heated to 90 ℃ in water-bath, then ethyl cellulose, Viscotrol C and tensio-active agent is added described Terpineol 350 and obtain the Terpineol 350 carrier, described Terpineol 350, ethyl cellulose, Viscotrol C and tensio-active agent mass percent are:
Terpineol 350 84.2%～94.2%,
Ethyl cellulose 4.0%～5.0%,
Viscotrol C 3.2%～4.2%,
Tensio-active agent 2.1%～3.1%;
Step 3, described glass is coated after raw material mixes with described Terpineol 350 carrier and be stirred to it and dissolve fully, thereby be cooled to room temperature formation paste carrier; Described glass coats raw material and Terpineol 350 carrier mass percent is:
Terpineol 350 carrier 65%～85%,
Glass coats raw material 15%～35%;
Step 4, cobalt sesquioxide, Manganse Dioxide, silicon-dioxide, nickel oxide and chromium sesquioxide are doped in the Zinc oxide powder, the purity of its each component is all greater than 99.95%, and described zinc oxide, cobalt sesquioxide, Manganse Dioxide, silicon-dioxide, nickel oxide and chromium sesquioxide mass percent are:
Zinc oxide 93 %～97 %,
Cobalt sesquioxide 0.5%～0.7%,
Manganse Dioxide 1.2%～1.6%,
Silicon-dioxide 0.5%～0.7%,
Nickel oxide 0.6%～0.8%,
Chromium sesquioxide 1.5%～1.9%;
Step 6, be that the aluminum particle of 0.5 ~ 1.5 μ m is put into electric furnace and obtained the surface by the abundant aluminum particle of oxidation with middle particle diameter;
Step 7, the Zinc oxide particles of described semiconductor and aluminum particle are non-conductively put into described paste carrier mutually with inorganic, and be heated to 60 ℃, stirred simultaneously 4 hours; Described inorganic non-conductive mutually in particle diameter be 0.1 ~ 0.3 μ m, this inorganic non-conductive be Al mutually
2O
3, SiO
2, CaO, any one among the MgO or their any mixture; The Zinc oxide particles of described semiconductor, aluminum particle, inorganic non-conductive phase and paste carrier mass percent are:
Zinc oxide particles 49.5 %～59.5% of semiconductor,
Aluminum particle 12.8%～16.8 %,
Inorganic non-conductive phase 2.8～3.2%,
Paste carrier 25.7%～29.7%;
Step 8, the mixture that adopts three-roll grinder that step 7 is made promptly get the anti-electrostatic slurry after disperseing, and this anti-electrostatic pulp particle fineness is less than 10 μ m.
Related content in the technique scheme is explained as follows:
1, in the such scheme, the scattered anti-electrostatic slurry of three-roll grinder passes through vacuum filtration in the described step 8, thereby removes the bubble in this slurry.
2, in the such scheme, in the described step 2, earlier will described ethyl cellulose add in the Terpineol 350 and stir, treat that it dissolves the back fully and dissolves fully adding Viscotrol C and tensio-active agent and be stirred to it.
3, in the such scheme, in the described step 3, described glass coats raw material to be mixed when the temperature of described Terpineol 350 carrier is 60 ℃.
4, in the such scheme, in the described step 6, described aluminum particle oxidation was warming up to 450 ℃ in 2 hours in electric furnace, form under the condition that is incubated 24 hours.
Because the technique scheme utilization, the present invention compared with prior art has following advantage and effect:
Zinc oxide surface of the present invention coats the insulating glass layer of one deck 10 ~ 200nm, can significantly improve its anti-electrostatic impact ability, below the near 1 μ A of the leakage current of normal operating conditions; Secondly, the present invention has the thixotropy that inorganic non-conductive phase has improved slurry greatly, can reduce the electric leakage of material; Once more, the aluminum particle that the present invention adopts the surface to have aluminum oxide can be regulated its static trigger voltage, can reduce the electric leakage of material simultaneously behind the aluminium powder oxidation, also can design different voltage breakdowns according to the application scenario.
Description of drawings
Fig. 1 is a zinc oxide material microcosmic synoptic diagram of the present invention.
In the above accompanying drawing: 1, Zinc oxide particles; 2, glass coating layer; 3, aluminum particle; 4, aluminium powder oxidation layer; 5, inorganic non-conductive phase.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment 1～5: a kind of slurry preparation method that is used for electrostatic devices may further comprise the steps:
Step 1, preparation glass coat raw material, and this glass coats the prescription of raw material mainly to be made up of the material of following quality percentage composition, as shown in table 1:
Table 1
| ? | Calcium isopropoxide | The boric acid tri butyl ester | Aluminum ethylate | Tetraethyl silicate resin |
| Embodiment 1 | 10% | 34% | 19% | 37% |
| Embodiment 2 | 12.5% | 31.5% | 26.5% | 29.5% |
| Embodiment 3 | 15% | 29% | 24% | 32% |
| Embodiment 4 | 17.5% | 26.5% | 21.5% | 34.5% |
| | 20% | 24% | 29% | 27% |
What the percentage sign in the table 1 was represented is the quality percentage composition.Annotate: calcium isopropoxide (((CH
3)
2CHO)
2Ca) be powder, the boric acid tri butyl ester is a powder, and aluminum ethylate is a powder, and tetraethyl silicate resin is a liquid.
Step 2, Terpineol 350 is heated to 90 ℃ in water-bath, then ethyl cellulose, Viscotrol C and tensio-active agent are added described Terpineol 350 and obtain the Terpineol 350 carrier, earlier will described ethyl cellulose add in the Terpineol 350 and stir, treat that it dissolves the back fully and dissolves fully adding Viscotrol C and tensio-active agent and be stirred to it; Described Terpineol 350, ethyl cellulose, Viscotrol C and tensio-active agent mass percent are as shown in table 2:
Table 2
| ? | Terpineol 350 | Ethyl cellulose | Viscotrol C | Tensio-active agent |
| Embodiment 1 | 87.2% | 6.5% | 1.7% | 4.6% |
| Embodiment 2 | 88.2% | 5.5% | 2.7% | 3.6% |
| Embodiment 3 | 89.2 % | 4.5% | 3.7% | 2.6% |
| Embodiment 4 | 90.2% | 3.5% | 4.7% | 1.6% |
| | 91.2% | 2.5% | 5.7% | 0.6% |
What the percentage sign in the table 2 was represented is the quality percentage composition.
Step 3, described glass is coated after raw material mixes with described Terpineol 350 carrier and be stirred to it and dissolve fully, thereby be cooled to room temperature formation paste carrier; Described glass coats raw material to be mixed when the temperature of described Terpineol 350 carrier is 60 ℃; Described glass coating raw material and Terpineol 350 carrier mass percent are as shown in table 2:
Table 3
| ? | The Terpineol 350 carrier | Glass coats raw material |
| Embodiment 1 | 65% | 35% |
| Embodiment 2 | 70% | 30% |
| Embodiment 3 | 75 % | 25% |
| Embodiment 4 | 80% | 20 |
| Embodiment | ||
| 5 | 85% | 15% |
What the percentage sign in the table 3 was represented is the quality percentage composition.
Step 4, cobalt sesquioxide, Manganse Dioxide, silicon-dioxide, nickel oxide and chromium sesquioxide are doped in the Zinc oxide powder, the purity of its each component is all greater than 99.95%, and described zinc oxide, cobalt sesquioxide, Manganse Dioxide, silicon-dioxide, nickel oxide and chromium sesquioxide mass percent are as shown in table 2:
Table 4
What the percentage sign in the table 4 was represented is the quality percentage composition.
Step 6, be that the aluminum particle 3 of 0.5 ~ 1.5 μ m is put into electric furnace and obtained the surface by the abundant aluminum particle 3 of oxidation with middle particle diameter; Described aluminum particle 3 oxidations were warming up to 450 ℃ in 2 hours in electric furnace, form under the condition that is incubated 24 hours;
Step 7, the Zinc oxide particles 1 of described semiconductor and aluminum particle 3 non-conductively 5 are put into described paste carrier mutually with inorganic, and be heated to 60 ℃, stirred simultaneously 4 hours; Particle diameter is 0.1 ~ 0.3 μ m in the described inorganic non-conductive phase 5, and this inorganic non-conductive phase 5 is Al
2O
3, SiO
2, CaO, any one among the MgO or their any mixture; The Zinc oxide particles 1 of described semiconductor, aluminum particle 3, inorganic non-conductive phase 5 and paste carrier mass percent are as shown in table 5:
Table 5
| ? | Terpineol 350 | Ethyl cellulose | Viscotrol C | Tensio-active agent |
| Embodiment 1 | 49.5 % | 19.8 % | 1% | 29.7% |
| Embodiment 2 | 52% | 17.3% | 2% | 28.7% |
| Embodiment 3 | 54.5 % | 14.8% | 3% | 27.7% |
| Embodiment 4 | 57% | 12.3% | 4% | 26.7 |
| Embodiment | ||||
| 5 | 59.5% | 9.8% | 5% | 25.7% |
What the percentage sign in the table 5 was represented is the quality percentage composition.
Step 8, the mixture that adopts three-roll grinder that step 7 is made promptly get the anti-electrostatic slurry after disperseing, and this anti-electrostatic pulp particle fineness is less than 10 μ m; The scattered anti-electrostatic slurry of three-roll grinder passes through vacuum filtration, thereby removes the bubble in this slurry.
Step 9, described anti-electrostatic slurry were handled through the following temperature rise period, thereby the zinc oxide of semiconductor, aluminum particle and inorganic non-conductive particle mutually interconnect by its surperficial glass coating layer 2.
Because the zinc oxide pressure-sensitive material has the leakage current of microampere order in normal operation, and after electrostatic impact, its leakage current has the trend that progressively increases.The present invention takes to coat at zinc oxide surface the insulating glass coating layer 2 of one deck 10 ~ 200nm, can significantly improve its anti-electrostatic impact ability, below the near 1 μ A of the leakage current of normal operating conditions.And the purposes of aluminium powder is to be used for regulating its static trigger voltage, and inorganic non-conductive phase 5 is the thixotropy that are used for improving slurry, and prevents that when sintering particulate of the same race from connecting.
The foregoing description only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (5)
1. slurry preparation method that is used for electrostatic devices is characterized in that: may further comprise the steps:
Step 1, preparation glass coat raw material, and this glass coats the prescription of raw material and mainly is made up of the material of following quality percentage composition:
Calcium isopropoxide, powder, 10%～20%,
The boric acid tri butyl ester, powder, 24%～34%,
Aluminum ethylate, powder, 19%～29%,
Tetraethyl silicate resin, liquid, 27%～37%;
Step 2, Terpineol 350 is heated to 90 ℃ in water-bath, then ethyl cellulose, Viscotrol C and tensio-active agent are added described Terpineol 350 and obtain the Terpineol 350 carrier, each constituent mass per-cent of Terpineol 350, ethyl cellulose, Viscotrol C and tensio-active agent is in the described Terpineol 350 carrier:
Terpineol 350 87.2%～91.2%,
Ethyl cellulose 2.5%～6.5%,
Viscotrol C 1.7%～5.7%,
Tensio-active agent 0.6%～4.6%;
Step 3, described glass is coated after raw material mixes with described Terpineol 350 carrier and be stirred to it and dissolve fully, thereby be cooled to room temperature formation paste carrier; Described glass coats raw material and Terpineol 350 carrier mass percent is:
Terpineol 350 carrier 65%～85%,
Glass coats raw material 15%～35%;
Step 4, cobalt sesquioxide, Manganse Dioxide, silicon-dioxide, nickel oxide and chromium sesquioxide are doped in the Zinc oxide powder, the purity of its each component is all greater than 99.95%, and described zinc oxide, cobalt sesquioxide, Manganse Dioxide, silicon-dioxide, nickel oxide and chromium sesquioxide mass percent are:
Zinc oxide 94 %～96%,
Cobalt sesquioxide 0.5%～0.7%,
Manganse Dioxide 0.4%～2.4%,
Silicon-dioxide 0.5%～0.7%,
Nickel oxide 0.6%～0.8%,
Chromium sesquioxide 1.6%～1.8%;
Step 5, with described adulterated Zinc oxide powder by ball-milling technology ball milling 48 hours, oven dry back granulation, briquetting, calcine down at 1200 ℃ then and obtained the pre-burning block in 4 hours, pre-burning block after will calcining again is through Mechanical Crushing, put into ball grinder ball milling 24 hours again, particle diameter is the Zinc oxide particles of the semiconductor of 1 μ m in promptly obtaining after the oven dry obtaining;
Step 6, be that the aluminum particle of 0.5 ~ 1.5 μ m is put into electric furnace and obtained the surface by the abundant aluminum particle of oxidation with middle particle diameter;
Step 7, the Zinc oxide particles of described semiconductor and aluminum particle are non-conductively put into described paste carrier mutually with inorganic, and be heated to 60 ℃, stirred simultaneously 4 hours; Described inorganic non-conductive mutually in particle diameter be 0.1 ~ 0.3 μ m, this inorganic non-conductive be Al mutually
2O
3, SiO
2, CaO, any one among the MgO or their any mixture; The Zinc oxide particles of described semiconductor, aluminum particle, inorganic non-conductive phase and paste carrier mass percent are:
Zinc oxide particles 49.5 %～59.5% of semiconductor,
Aluminum particle 9.8%～19.8 %,
Inorganic non-conductive phase 1～5%,
Paste carrier 25.7%～29.7%;
Step 8, the mixture that adopts three-roll grinder that step 7 is made promptly get the anti-electrostatic slurry after disperseing, and this anti-electrostatic pulp particle fineness is less than 10 μ m.
2. slurry preparation method according to claim 1 is characterized in that: the scattered anti-electrostatic slurry of three-roll grinder passes through vacuum filtration in the described step 8, thereby removes the bubble in this slurry.
3. slurry preparation method according to claim 1 is characterized in that: in the described step 2, earlier will described ethyl cellulose add in the Terpineol 350 and stir, treat that it dissolves the back fully and dissolves fully adding Viscotrol C and tensio-active agent and be stirred to it.
4. slurry preparation method according to claim 1 is characterized in that: in the described step 3, described glass coats raw material to be mixed when the temperature of described Terpineol 350 carrier is 60 ℃.
5. slurry preparation method according to claim 1 is characterized in that: in the described step 6, described aluminum particle oxidation was warming up to 450 ℃ in 2 hours in electric furnace, form under the condition that is incubated 24 hours.
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| CN107629466A (en) * | 2017-09-20 | 2018-01-26 | 苏州晶讯科技股份有限公司 | A kind of function slurry for chip macromolecule static suppressor |
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| CN107629466A (en) * | 2017-09-20 | 2018-01-26 | 苏州晶讯科技股份有限公司 | A kind of function slurry for chip macromolecule static suppressor |
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| CN102220109B (en) | 2013-10-02 |
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