CN109326401A - A kind of preparation process of nano zinc oxide composite powder piezoresistive wafer - Google Patents
A kind of preparation process of nano zinc oxide composite powder piezoresistive wafer Download PDFInfo
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- CN109326401A CN109326401A CN201811325969.0A CN201811325969A CN109326401A CN 109326401 A CN109326401 A CN 109326401A CN 201811325969 A CN201811325969 A CN 201811325969A CN 109326401 A CN109326401 A CN 109326401A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/006—Apparatus or processes specially adapted for manufacturing resistors adapted for manufacturing resistor chips
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/28—Apparatus or processes specially adapted for manufacturing resistors adapted for applying terminals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/30—Apparatus or processes specially adapted for manufacturing resistors adapted for baking
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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
- H01C7/112—ZnO type
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Abstract
The invention discloses a kind of preparation processes of nano zinc oxide composite powder piezoresistive wafer, belong to electron ceramic material preparation and applied technical field, insulation glaze is applied by the preparation of nano zinc oxide composite powder, aqueous, tabletting, sintering, grinding, cleaning, aluminium-plated, side, obtains nano zinc oxide composite powder piezoresistive wafer.Present invention process preparation process is simple, it is raw materials used cheap and easily-available, equipment operation is simple, accurately control stoichiometric ratio, product purity is high, it can carry out atom, molecular level mixing, zinc oxide composite powder grain diameter obtained is smaller, and uniform component distribution, nano zinc oxide composite powder of the present invention prepares resistor disc process and needs not move through ball milling, prilling, without adhesive polyethylene alcohol is added, crude green body made from tabletting is also able to maintain good intensity, slight crack will not occur in calcining, energy consumption is lower, reduce production cost, and it is environmentally friendly, both production efficiency can be improved, be conducive to mass production.
Description
Technical field
The invention belongs to electron ceramic material preparation and applied technical fields, are related to a kind of nano zinc oxide composite powder pressure
The preparation process of quick resistor disc.
Background technique
With the progress of modern electronic technology, so that commercial equipment develops towards device miniaturization direction.In addition, with
The construction of extra-high voltage, so that the zinc oxide valve plate volume and quality for arrester are significantly increased.In order to reduce zinc oxide valve plate
Volume and quality, make its miniaturization, then need the voltage gradient for improving Zinc-oxide piezoresistor, and this requires prepare resistor disc
Zinc oxide compound powder end particle nanosizing used and its component, microstructure homogenization.
The process of preparing of production zinc oxide piezoresistor composite powder is mainly solid phase mechanical attrition method at present, although
Solid phase method is easy to operate, and cost is relatively low, it can be difficult to acquisition component is uniform, the lesser composite granule of grain diameter.The study found that
The main reason for influencing resistor disc through-current capability is that the microcosmic unevenness structure of resistor disc powder leads to the unevenness of current distribution,
Resulting heat causes built-in thermal stress to be formed, so that resistor disc be made to puncture or burst.In addition, the voltage gradient of resistor disc
Related with the composition particle size of resistor disc particle, the partial size of particle is smaller, and the voltage gradient of resistor disc is bigger.
The technological process of production of existing zinc oxide varistor are as follows: ingredient, grinding, granulation, aqueous, tabletting, sintering, mill
Piece cleaning, aluminium-plated upper side insulating layer, finally obtain zinc oxide varistor, technique is cumbersome, and the production cycle is long, production efficiency
It is lower；Generally use ball-milling technology, the partial size of particle is larger after ball milling, mixing it is ineffective, it is difficult to obtain nanoscale original
Feed powder end；And need to add binder polyvinyl alcohol into slurry when being granulated, it can decompose to obtain in sintering
CO2、H2O and carbon black increase the porosity of zinc oxide resistance sheet, reduce the homogeneity of resistor disc internal structure；It increases simultaneously
Production cost is unfavorable for the safety in production of operator, can also generate dirt to environment since polyvinyl alcohol has chemical toxicity
Dye.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of nano zinc oxide composite powder varistors
The preparation process of piece, to be prepared, grain diameter is small, component is uniform, environmentally friendly, voltage gradient is high and negotiability
Strong zinc oxide composite powder piezoresistive wafer.
The preparation process of this nano zinc oxide composite powder piezoresistive wafer provided by the invention, comprising the following steps:
(1) zinc salt, cobalt salt, chromic salts and boric acid are made into aqueous solution by preset ratio, are slowly added to citric acid thereto
Dispersion is stirred at room temperature in the ethylene glycol solution of aqueous solution and bismuth salt, antimonic salt, obtains metal mixed salt solution；
(2) metal mixed salt solution is subjected to isothermal holding at a set temperature, obtains wet gel, wet gel is dried
Dry-cure obtains xerogel；
(3) xerogel is placed in Muffle furnace, is calcined at a predetermined temperature, calcined product is ground,
Then after washed, drying, nano zinc oxide composite powder is obtained；
(4) aqueous: the distilled water of predetermined amount being added into nano zinc oxide composite powder, stirs, is contained
Powder after water；
(5) tabletting: the powder after will be aqueous, which is put into tablet press machine, is compressed into tablet form crude green body；
(6) be sintered: by crude green body in Muffle furnace calcination processing；
(7) it is ground, cleans: resistor disc grinding two end surfaces are cleaned up using distilled water；
(8) aluminium-plated, side applies insulation glaze: resistor disc both ends of the surface being sprayed aluminium electrode, insulation glaze is applied in side, obtains nanometer
Zinc oxide composite powder piezoresistive wafer.
Preferably, in the metal mixed salt solution, zinc salt: 85~95mol%, 1~5mol% of cobalt salt, chromic salts 0~
5mol%, 1~5mol% of boric acid, 0~5mol% of bismuth salt, 2~5mol% of antimonic salt, the sum of molar percentage of each component are
100mol%.
Preferably, the molar concentration of zinc salt is 0.5~3mol/L, and citric acid rubs in the metal mixed salt solution
Your concentration is 0~2mol/L, and the molar concentration of ethylene glycol is 2~10mol/L.
Preferably, the metal salt is one of nitrate, acetate, chlorate or a variety of.
Preferably, metal mixed salt solution carries out isothermal holding in 70~100 DEG C of water-bath in the step (2),
Soaking time is 12~36h.
Preferably, in the step (2), the drying temperature of wet gel is 120~180 DEG C, drying time is 24~
48h。
Preferably, calcination temperature is 350~600 DEG C in the step (3), soaking time is 2~4h.
Preferably, using mortar grinder calcined product, milling time is 2~10min in the step (3).
Preferably, washed in the step (3) using deionized water and dehydrated alcohol, deionized water with it is anhydrous
The dosage of ethyl alcohol and the volume mass ratio of nano zinc oxide composite powder are 10~30ml/g.
Preferably, the steaming of 1~1.5% mass fraction is added into nano zinc oxide composite powder in the step (4)
Distilled water.
Preferably, calcination temperature is 900~1150 DEG C in the step (6), soaking time is 1~5h.
The present invention also provides be prepared according to the preparation process of the nano zinc oxide composite powder piezoresistive wafer
Nano zinc oxide composite powder piezoresistive wafer.
The principle of the present invention: the present invention prepares nano zinc oxide composite powder using improved Pechini method, and metal salt is mixed
Closing in solution includes boric acid, citric acid and ethylene glycol solution, is conducive to the dispersion of particle, prevents particle aggregation from growing up, from molecule
Level mixes each component uniformly, particle nanosizing, because without ball milling, gel uses lower calcination temperature in calcining
So that retaining part of hydroxyl in composite granule, since there are hydrogen bonds between hydroxyl and hydroxyl, powder can be enhanced in (350~600 DEG C)
Interaction between body, therefore do not have to that adhesive polyethylene alcohol is added, it does not need to be granulated, directly by nano zinc oxide composite powder
Crude green body made from aqueous, tabletting is also able to maintain good intensity, is not in slight crack in calcining, due to being free of polyvinyl alcohol,
CO will not be generated when sintering2、H2O and carbon black, reduce the porosity of zinc oxide resistance sheet, the distributing homogeneity of resistor disc each component,
To improve the electric potential gradient, through-current capability and tolerance high current impulse withstanding capability of zinc oxide resistance sheet.
Compared with the existing technology, the present invention has following advantageous effects:
The preparation process of nano zinc oxide composite powder piezoresistive wafer of the present invention, preparation process is simple, used
Raw material is cheap and easily-available, and equipment operation is simple, accurately controls stoichiometric ratio, and product purity is high, and it is mixed can to carry out atom, molecular level
It closes, zinc oxide composite powder grain diameter obtained is smaller, and uniform component distribution, nano zinc oxide composite powder of the present invention
It prepares resistor disc process and needs not move through ball milling, prilling, do not have to that adhesive polyethylene alcohol, crude green body made from tabletting is added
It is able to maintain good intensity, slight crack will not occur in calcining, energy consumption is lower, reduces production cost, and environmentally friendly, both
Production efficiency can be improved, be conducive to mass production, and improved the electric property of zinc oxide resistance sheet, had extensive
Application prospect.
For the present invention using deionized water and ethylene glycol as solvent, citric acid is complexing agent, and citric acid has strong coordination ability,
Carboxyl in citric acid can form complex compound with different metal ions simultaneously from hydroxyl, so that cation is reached molecular level mixed
It closes；And ethylene glycol can also play Ligands and dispersing agent effect wherein, can promote the dissolution and stabilization of metal ion
Complexing；Reinforce the complexing to metal ion by citric acid and ethylene glycol collective effect, utilizes the ester between the two functional group
Hydrogen bond action between change effect and complex molecule obtains bigger stabilization reticular structure, is distributed cation in presoma more
It is even, more stable.Relative to other wet chemistry methods preparation zinc oxide composite powder, operation of the present invention is simpler, component with
And particle size distribution is more uniform.
Detailed description of the invention
Fig. 1 is the preparation technology flow chart of 1 nano zinc oxide composite powder piezoresistive wafer of the embodiment of the present invention.
Fig. 2 is that the SEM of 1 gained nano zinc oxide composite powder resistor disc of the embodiment of the present invention schemes.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, rather than whole embodiments, based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
Experimental method described in following embodiments is unless otherwise specified conventional method, the reagent and material, such as
Without specified otherwise, commercially obtain.
Embodiment 1
The raw material of the present embodiment is prepared by following molar percentage, and specific formula is as follows:
Zinc salt: 90.2mol%, cobalt salt 2.59mol%, boric acid 1.93mol%, bismuth salt 1.98mol%, antimonic salt
3.3mol%.
A kind of preparation process of nano zinc oxide composite powder piezoresistive wafer of the present invention, it is specific as shown in Figure 1, include with
Lower step:
(1) 165.5g zinc acetate, 7.5g cabaltous nitrate hexahydrate, 1.2g boric acid is weighed to be dissolved in 400ml deionized water and stirring
Form red, transparent solution；45.3g citric acid is weighed to be dissolved in ultrasonic disperse in 350ml deionized water to form transparent citric acid molten
Liquid；Weigh that 7.8g bismuth nitrate, that 7.5g antimony chloride is dissolved in ultrasonic disperse in 250ml ethylene glycol is transparent to solution；By transparent lemon
Acid solution, bismuth salt antimonic salt ethylene glycol solution in being respectively added slowly in acetic acid zinc solution in 20min, stir evenly to form gold
Belong to mixed salt solution；
(2) metal mixed salt solution is put into keep the temperature in 80 DEG C of constant temperature pot and forms stable wet gel for 24 hours, it will be wet solidifying
Glue is put into electric drying oven with forced convection, is toasted for 24 hours under 120 DEG C of environment, is then toasted under 180 DEG C of environment for 24 hours, is obtained dry solidifying
Glue；
(3) xerogel is put into tube furnace and is calcined, heating rate 3 DEG C/min, 200 DEG C of heat preservation 2h are then proceeded to
Be warming up under 450 DEG C of environment and calcine 2h, calcined product is ground into 5min using agate mortar, by obtained composite granule spend from
Sub- water and alcohol washes respectively twice, the volume mass of the dosage and nano zinc oxide composite powder of deionized water and dehydrated alcohol
Than for 20ml/g, detailed process are as follows: pour into deionized water into the beaker equipped with zinc oxide composite powder, stirred with glass bar
1min stands 4h, upper water is outwelled, and filters, and is re-poured into deionized water cleaning, so repeats；
Cleaned zinc oxide composite powder is put into electric drying oven with forced convection, drying for 24 hours, is received in 80 DEG C of environment
Rice zinc oxide composite powder；
(4) aqueous: the distilled water of 1.5wt% being added into nano zinc oxide composite powder, stirs, is contained
Powder after water；
(5) tabletting: the powder after will be aqueous, which is put into tablet press machine, is compressed into tablet form crude green body；
(6) be sintered: by crude green body in Muffle furnace calcination processing；2 DEG C/h of heating rate is warming up to 1050 DEG C, keeps the temperature 2h, drop
Warm 3 DEG C/h of rate；
(7) it is ground, cleans: resistor disc grinding two end surfaces are cleaned up using distilled water；
(8) aluminium-plated, side applies insulation glaze: resistor disc both ends of the surface being sprayed aluminium electrode, insulation glaze is applied in side, obtains nanometer
Zinc oxide composite powder piezoresistive wafer, SEM scheme as shown in Fig. 2, as can be seen from Fig., resistor disc component is uniform, zinc oxide
In the form of sheets, partial size is smaller.
(outer ring is straight for the piezoresistive wafer that the specification of nano zinc oxide composite powder piezoresistive wafer is Φ 70 in embodiment 1
Diameter is 72mm, annular diameters 26mm, is highly 22.5mm), the test gained voltage gradient of piezoresistive wafer, through-current capability and
It is resistant to high current impulse withstanding capability, as shown in table 1.
Embodiment 2
The raw material of the present embodiment is prepared by following molar percentage, and specific formula is as follows:
Zinc salt: 89.5mol%, cobalt salt 1.3mol%, chromic salts 1.1mol%, boric acid 1.6mol%, bismuth salt 3.2mol%, antimony
Salt 3.3mol%.
A kind of preparation process of nano zinc oxide composite powder piezoresistive wafer of the present invention, comprising the following steps:
(1) 266.3g zinc nitrate hexahydrate, 3.8g cobalt nitrate, 2.6g chromic nitrate, 1g boric acid are weighed and is dissolved in 400ml deionization
Stirring forms red, transparent solution in water；Weighing 50g citric acid is dissolved in ultrasonic disperse in 350ml deionized water and forms transparent lemon
Lemon acid solution；Weigh that 12.4g bismuth acetate, that 7.53g antimony chloride is dissolved in ultrasonic disperse in 250ml ethylene glycol is transparent to solution；It will be saturating
For the ethylene glycol solution of bright citric acid solution, bismuth salt antimonic salt in being respectively added slowly in acetic acid zinc solution in 20min, stirring is equal
Even formation metal mixed salt solution；
(2) metal mixed salt solution is put into 90 DEG C of constant temperature pot and keeps the temperature 16h, form stable wet gel, it will be wet solidifying
Glue is put into electric drying oven with forced convection, is toasted for 24 hours under 120 DEG C of environment, is then toasted under 180 DEG C of environment for 24 hours, is obtained dry solidifying
Glue；
(3) xerogel is put into tube furnace and is calcined, heating rate 3 DEG C/min, 200 DEG C of heat preservation 2h are then proceeded to
Be warming up under 400 DEG C of environment and calcine 3h, calcined product is ground into 5min using agate mortar, by obtained composite granule spend from
Sub- water and alcohol washes respectively twice, the volume mass of the dosage and nano zinc oxide composite powder of deionized water and dehydrated alcohol
Than for 10ml/g, detailed process are as follows: pour into deionized water into the beaker equipped with zinc oxide composite powder, stirred with glass bar
1min stands 4h, upper water is outwelled, and filters, and is re-poured into deionized water cleaning, so repeats；
Cleaned zinc oxide composite powder is put into electric drying oven with forced convection, drying for 24 hours, is received in 80 DEG C of environment
Rice zinc oxide composite powder；
(4) aqueous: the distilled water of 1.0wt% being added into nano zinc oxide composite powder, stirs, is contained
Powder after water；
(5) tabletting: the powder after will be aqueous, which is put into tablet press machine, is compressed into tablet form crude green body；
(6) be sintered: by crude green body in Muffle furnace calcination processing；2 DEG C/h of heating rate is warming up to 1050 DEG C, keeps the temperature 2h, drop
Warm 2 DEG C/h of rate；
(7) it is ground, cleans: resistor disc grinding two end surfaces are cleaned up using distilled water；
(8) aluminium-plated, side applies insulation glaze: resistor disc both ends of the surface being sprayed aluminium electrode, insulation glaze is applied in side, obtains nanometer
Zinc oxide composite powder piezoresistive wafer.
(outer ring is straight for the piezoresistive wafer that the specification of nano zinc oxide composite powder piezoresistive wafer is Φ 70 in embodiment 2
Diameter is 72mm, annular diameters 26mm, is highly 22.5mm), the test gained voltage gradient of piezoresistive wafer, through-current capability and
It is resistant to high current impulse withstanding capability, as shown in table 1.
Embodiment 3
The raw material of the present embodiment is prepared by following molar percentage, and specific formula is as follows:
Zinc salt: 90.2mol%, cobalt salt 1.1mo%, chromic salts 0.5mol%, boric acid 1.2mol%, bismuth salt 3.1mol%, antimony
Salt 3.9mol%.
A kind of preparation process of nano zinc oxide composite powder piezoresistive wafer of the present invention, comprising the following steps:
(1) 165.5g zinc acetate, 1.9g cobalt acetate, 1.1g chromium acetate, 0.7g boric acid is weighed to be dissolved in 400ml deionized water
Stirring forms red, transparent solution；Weighing 62g citric acid is dissolved in ultrasonic disperse in 350ml deionized water and forms transparent citric acid
Solution；Weigh that 12.2g bismuth nitrate, that 12.0g nitric acid antimony is dissolved in ultrasonic disperse in 250ml ethylene glycol is transparent to solution；It will be transparent
Citric acid solution, bismuth salt antimonic salt ethylene glycol solution in being respectively added slowly in acetic acid zinc solution in 20min, stir evenly shape
At metal mixed salt solution；
(2) metal mixed salt solution is put into 100 DEG C of constant temperature pot and keeps the temperature 12h, form stable wet gel, it will be wet solidifying
Glue is put into electric drying oven with forced convection, is toasted for 24 hours under 120 DEG C of environment, is then toasted under 180 DEG C of environment for 24 hours, is obtained dry solidifying
Glue；
(3) xerogel is put into tube furnace and is calcined, heating rate 3 DEG C/min, 200 DEG C of heat preservation 2h are then proceeded to
Be warming up under 500 DEG C of environment and calcine 2h, calcined product is ground into 5min using agate mortar, by obtained composite granule spend from
Sub- water and alcohol washes respectively twice, the volume mass of the dosage and nano zinc oxide composite powder of deionized water and dehydrated alcohol
Than for 30ml/g, detailed process are as follows: pour into deionized water into the beaker equipped with zinc oxide composite powder, stirred with glass bar
1min stands 4h, upper water is outwelled, and filters, and is re-poured into deionized water cleaning, so repeats；
Cleaned zinc oxide composite powder is put into electric drying oven with forced convection, drying for 24 hours, is received in 80 DEG C of environment
Rice zinc oxide composite powder；
(4) aqueous: the distilled water of 1.5wt% being added into nano zinc oxide composite powder, stirs, is contained
Powder after water；
(5) tabletting: the powder after will be aqueous, which is put into tablet press machine, is compressed into tablet form crude green body；
(6) be sintered: by crude green body in Muffle furnace calcination processing；3 DEG C/h of heating rate is warming up to 1000 DEG C, keeps the temperature 2h, drop
Warm 2 DEG C/h of rate；
(7) it is ground, cleans: resistor disc grinding two end surfaces are cleaned up using distilled water；
(8) aluminium-plated, side applies insulation glaze: resistor disc both ends of the surface being sprayed aluminium electrode, insulation glaze is applied in side, obtains nanometer
Zinc oxide composite powder piezoresistive wafer.
(outer ring is straight for the piezoresistive wafer that the specification of nano zinc oxide composite powder piezoresistive wafer is Φ 70 in embodiment 3
Diameter is 72mm, annular diameters 26mm, is highly 22.5mm), the test gained voltage gradient of piezoresistive wafer, through-current capability and
It is resistant to high current impulse withstanding capability, as shown in table 1.
Comparative example 1
Using the preparation method for the Zinc oxide-base composite granule resistor disc that common ball grinding method obtains, including walk as follows
It is rapid:
(1) raw material is prepared:
Weigh 161.5g zinc oxide, 4.2g cobalt oxide, 1.6g chromium oxide, 0.2g boron oxide, 21.6g bismuth oxide, 10.8g oxygen
Change antimony, is put into ball mill and grinds 2h, obtain mixed powder；
(2) it grinds: mixed powder being added in the distilled water of 50% mass fraction and stirred evenly, is then placed in sand mill
Grind 12h；
(3) it is granulated: the polyvinyl alcohol of 5% mass fraction being added into the slurry after grinding, is then placed in pelletizer and sprays
Mist is granulated；
(4) aqueous: the distilled water of 1.5% mass fraction being added into the powder after granulation, stirs；
(5) tabletting: the powder after will be aqueous, which is put into tablet press machine, is compressed into tablet form crude green body；
(6) be sintered: by crude green body in Muffle furnace calcination processing；2 DEG C/h of heating rate is warming up to 1100 DEG C, keeps the temperature 2h, drop
Warm 3 DEG C/h of rate；
(7) it is ground, cleans: resistor disc both ends being polished, are cleaned up using distilled water；
(8) aluminium-plated, side applies insulation glaze: resistor disc both ends being sprayed aluminium electrode, insulation glaze is applied in side, obtains zinc oxide
Composite granule piezoresistive wafer.
(outer annular diameter is for the specification of zinc oxide composite powder piezoresistive wafer is Φ 70 in comparative example 1 piezoresistive wafer
72mm, annular diameters 26mm are highly 22.5mm), voltage gradient, through-current capability and the tolerance of test gained piezoresistive wafer
High current impulse withstanding capability, as shown in table 1.
The comparison of 1 zinc oxide composite powder piezoresistive wafer electric property of table
As it can be seen from table 1 through the invention technique synthesis zinc oxide composite powder piezoresistive wafer, compared to it is common
Resistor disc made from ball-milling technology (comparative example 1), electric potential gradient, through-current capability and tolerance high current impulse withstanding capability and routine side
Zinc oxide resistance sheet made from method illustrates that the nano zine oxide of the technique provided through the invention synthesis is multiple compared to being obviously improved
Powder is closed compared with the Zinc oxide-base composite granule that common ball-milling method obtains with ingredient and smaller partial size more evenly；
Ball milling, prilling are needed not move through during nano zinc oxide composite powder piezoresistive wafer provided by the invention, is not required to
Adhesive polyethylene alcohol is added, manufactured Nanocrystalline Zno-based Varistor piece still has good performance, not only reduces life
Cost is produced, and improves production efficiency, entire production process is environmentally friendly.
Claims (10)
1. a kind of preparation process of nano zinc oxide composite powder piezoresistive wafer, which comprises the following steps:
(1) zinc salt, cobalt salt, chromic salts and boric acid are made into aqueous solution by preset ratio, are slowly added to the water-soluble of citric acid thereto
Dispersion is stirred at room temperature in the ethylene glycol solution of liquid and bismuth salt, antimonic salt, obtains metal mixed salt solution；
(2) metal mixed salt solution is subjected to isothermal holding at a set temperature, obtains wet gel, wet gel is carried out at drying
Reason, obtains xerogel；
(3) xerogel is placed in Muffle furnace, is calcined at a predetermined temperature, calcined product is ground, then
After washed, drying, nano zinc oxide composite powder is obtained；
(4) aqueous: into nano zinc oxide composite powder be added predetermined amount distilled water, stir, obtain it is aqueous after
Powder；
(5) tabletting: the powder after will be aqueous, which is put into tablet press machine, is compressed into tablet form crude green body；
(6) be sintered: by crude green body in Muffle furnace calcination processing；
(7) it is ground, cleans: resistor disc grinding two end surfaces are cleaned up using distilled water；
(8) aluminium-plated, side applies insulation glaze: resistor disc both ends of the surface being sprayed aluminium electrode, insulation glaze is applied in side, obtains nano oxidized
Zinc composite granule piezoresistive wafer.
2. the preparation process of nano zinc oxide composite powder piezoresistive wafer according to claim 1, which is characterized in that described
In metal mixed salt solution, zinc salt: 85~95mol%, 1~5mol% of cobalt salt, 0~5mol% of chromic salts, 1~5mol% of boric acid,
0~5mol% of bismuth salt, 2~5mol% of antimonic salt, the sum of molar percentage of each component are 100mol%.
3. the preparation process of nano zinc oxide composite powder piezoresistive wafer according to claim 1 or claim 2, which is characterized in that
In the metal mixed salt solution, the molar concentration of zinc salt is 0.5~3mol/L, and the molar concentration of citric acid is 0~2mol/L,
The molar concentration of ethylene glycol is 2~10mol/L.
4. the preparation process of nano zinc oxide composite powder piezoresistive wafer according to claim 1 or claim 2, which is characterized in that
The metal salt is one of nitrate, acetate, chlorate or a variety of.
5. the preparation process of nano zinc oxide composite powder piezoresistive wafer according to claim 1, which is characterized in that described
In step (2), metal mixed salt solution carries out isothermal holding in 70~100 DEG C of water-bath, and soaking time is 12~36h.
6. the preparation process of nano zinc oxide composite powder piezoresistive wafer according to claim 1, which is characterized in that described
In step (2), the drying temperature of wet gel is 120~180 DEG C, and drying time is 24~48h.
7. the preparation process of nano zinc oxide composite powder piezoresistive wafer according to claim 1, which is characterized in that described
In step (3), calcination temperature is 350~600 DEG C, and soaking time is 2~4h.
8. the preparation process of nano zinc oxide composite powder piezoresistive wafer according to claim 1, which is characterized in that described
In step (4), the distilled water of 1~1.5% mass fraction is added into nano zinc oxide composite powder.
9. the preparation process of nano zinc oxide composite powder piezoresistive wafer according to claim 1, which is characterized in that described
In step (6), calcination temperature is 900~1150 DEG C, and soaking time is 1~5h.
10. it is a kind of according to claim 1~any one of 9 described in nano zinc oxide composite powder piezoresistive wafer preparation process
The nano zinc oxide composite powder piezoresistive wafer being prepared.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205758A (en) * | 2020-02-26 | 2020-05-29 | 南京君弘新材料有限公司 | Transparent antistatic liquid and preparation method thereof |
| CN111508676A (en) * | 2020-04-24 | 2020-08-07 | 国网湖南省电力有限公司 | Small-size distribution network annular zinc oxide resistance card and preparation method thereof |
| CN112811893A (en) * | 2021-01-09 | 2021-05-18 | 浙江大学台州研究院 | Method for uniformly doping nanoparticles in high-temperature superconducting material |
| CN116835975A (en) * | 2023-07-05 | 2023-10-03 | 广东电网有限责任公司 | ZnO polycrystalline ceramic with high breakdown field strength, preparation method and cable sheath protector |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205758A (en) * | 2020-02-26 | 2020-05-29 | 南京君弘新材料有限公司 | Transparent antistatic liquid and preparation method thereof |
| CN111508676A (en) * | 2020-04-24 | 2020-08-07 | 国网湖南省电力有限公司 | Small-size distribution network annular zinc oxide resistance card and preparation method thereof |
| CN111508676B (en) * | 2020-04-24 | 2021-08-24 | 国网湖南省电力有限公司 | Small-size distribution network annular zinc oxide resistance card and preparation method thereof |
| CN112811893A (en) * | 2021-01-09 | 2021-05-18 | 浙江大学台州研究院 | Method for uniformly doping nanoparticles in high-temperature superconducting material |
| CN116835975A (en) * | 2023-07-05 | 2023-10-03 | 广东电网有限责任公司 | ZnO polycrystalline ceramic with high breakdown field strength, preparation method and cable sheath protector |
| CN116835975B (en) * | 2023-07-05 | 2024-05-14 | 广东电网有限责任公司 | ZnO polycrystalline ceramic with high breakdown field strength, preparation method and cable sheath protector |
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