CN110143817A - A kind of powder injection-molded PP Pipe Compound and preparation method of bismuth stearate cladding lead lanthanum zirconate titanate - Google Patents
A kind of powder injection-molded PP Pipe Compound and preparation method of bismuth stearate cladding lead lanthanum zirconate titanate Download PDFInfo
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Abstract
The present invention relates to the powder injection-molded PP Pipe Compounds and preparation method of a kind of bismuth stearate cladding lead lanthanum zirconate titanate, raw material including following component: PLZT powder 86.87~88.99%, polyethylene glycol 6.01~7.88%, polyvinyl butyral 2.00~2.62%, polyformaldehyde 2.00~2.62%, powder modifier 0.50~4.00%, surplus is lubricating auxiliary agent, the preparation method is to be surface-treated with bismuth stearate to PLZT powder, mixing is completed in mixer after ingredient, extruding pelletization and injection moulding after broken, porcelain is sintered into after completing first step degreasing in deionized water.The present invention, to the processing of PLZT powder cladding, reduces feeding viscosity, finished product compactness greatly improves after sintering, solves agglomeration traits of the fine powder in process of injection molding, and improve the dielectric constant and piezoelectric property of PLZT piezoelectric ceramics by bismuth stearate.
Description
Technical field
The present invention relates to powder injection molding technology and piezoelectric ceramics technologies of preparing more particularly to a kind of bismuth stearate to coat
The powder injection molding technology and preparation method of lead lanthanum zirconate titanate (PLZT).
Background technique
Powder injection-molded is a kind of novel near net to grow up on the basis of injection-moulding plastic and powder metallurgy
Forming technique.Using the mixture of metal or inorganic powder and binder as feeding, by injector certain pressure, temperature and
It is cooling to obtain injection green compact by the feeding injection mold cavity with flowable state under speed, after by degreasing, sintering and simple
Following process obtain finished product.Products surface quality is good, and density is high, and precision is high, it is easy to accomplish automated production.
The problems such as solid content is low, easy to reunite in injection moulding for fine powder, most common method are to utilize various tables
Face activating agent pre-processes powder.Surfactant can be roughly divided into two types: one kind is fatty acid (SA, OA, HSA),
By Lewis acid-base reaction Hydrogen Binding Adsorption on ceramic powders surface；Another kind of is coupling agent (silane, titanate), by covalent
Key is integrated on ceramic powder.They all can serve as the bridge between molten polymer and ceramic powders, improves ceramic powders and exists
Dispersion in adhesive, to increase the compatibility between adhesive component and reduce viscosity.
And for piezoelectric ceramics, the incorporation of the elements such as silicon, titanium may destroy original crystal structure, to piezoelectricity
Performance adversely affects.Bismuth is a kind of soft doped chemical of common piezoelectric ceramics, for improving piezoelectric property, reducing and burn
Junction temperature.It uses to this research and innovation bismuth stearate as powder modifier, improves the combination of powder and resin, improve injection
Base intensity and rheology, while it can generate nano bismuth oxide in piezoelectricity powder surface in heat-agglomerating, improve mixing for bismuth oxide
Miscellaneous efficiency.It is prepared for PLZT injection PP Pipe Compound using CIM technology, obtains low viscosity, better powder dispersity, and improve
The piezoelectric property of PLZT ceramics.Binder selects the environment-friendly type water degreasing binder based on PEG, both avoids organic solvent
Pollution, also specific heat degreasing efficiency is higher.
Summary of the invention
The technical problem to be solved by the present invention is provide a kind of bismuth stearate cladding PLZT powder injection molding technology and
Preparation method reduces feeding viscosity, finished product compactness mentions significantly after sintering by bismuth stearate to the processing of PLZT powder cladding
Height solves agglomeration traits of the fine powder in process of injection molding, prepares low viscosity, and the injection of height injection base intensity is dedicated
Material, and the doping efficiency of bismuth oxide can be improved, so that the piezoelectric property of PLZT piezoelectric ceramics improves, it is made to have more market competition
Power.
The present invention solves its technical problem and adopts the following technical solutions to realize.It is proposed according to the present invention a kind of hard
Resin acid bismuth coats the powder injection molding technology and preparation method of PLZT, and it includes following:
PLZT powder (lead lanthanum zirconate titanate), powder modifier bismuth stearate and binder, binder mainly by binder by
PEG, PVB, POM and lubricating auxiliary agent mixing composition；
The mass percent of above-mentioned each component is as follows: PLZT powder 86.87~88.99%, polyethylene glycol (PEG) 6.01~
7.88%, polyvinyl butyral (PVB) 2.00~2.62%, polyformaldehyde (POM) 2.00~2.62%, powder modifier 0.50
~4.00%, surplus is lubricating auxiliary agent.
Selected PLZT powder each group distribution ratio is:
Pb0.91La0.06(Zr0.58Ti0.42)0.975Nb0.02O3, wherein Pb3O4For 64.43%, La2O3For 3.03%, ZrO2For
21.59%, TiO2For 10.13% and Nb2O5It is 0.82%.
The powder modifier is bismuth stearate, is to be prepared using one-step method, i.e., by stearic acid heating melting
After put into Bi2O3, by stearic acid and Bi2O3Molar ratio 1:(0.47-0.49) it feeds intake, the glacial acetic acid of addition stearic acid dosage 3% is made
For catalyst, 2% isopropanol reacts two hours at 130 DEG C as foam in hibitors.
Reaction equation is as follows: Bi2O3+2C17H35COOH→2BiOC17H35CO2+H2O。
The binder system is environment friendly and pollution-free water-soluble degreasing system: water-soluble component PEG can moisten well
Smoothers end plays a part of reducing viscosity, has cracking solution rate in water, it is de- that the hole left after removing becomes heat
The channel for the micro-molecular gas evolution that residue binder decomposes when rouge；Guarantor type resin PVB due to the structure of side chain polyhydroxy and it is right
Powder coheres effect with good, but its softening temperature is lower, and POM has high-melting-point and high intensity, for improving green compact
Heat resisting temperature.
The PEG is the PEG mixture of different molecular weight, wherein PEG20000 and PEG1500 1:(2-3 in mass ratio) group
At low molecular weight PEG1500 is used for quick water degreasing, and high molecular weight PEGs 20000 are for obtaining higher powder loading.
The lubricating auxiliary agent is one of paraffin and polyethylene wax or mixture.
Bismuth stearate coats the preparation method of the powder injection-molded PP Pipe Compound of PLZT:
(1) preparation of PLZT powder: with Pb3O4、La2O3、ZrO2、TiO2And Nb2O5To prepare raw material, purity is all larger than
99%, in order to keep stoichiometry, all oxides are sufficiently dry before weighing, and raw material is after ball milling mixing is uniform in 850
DEG C calcining 2h PLZT powder, ball milling sieving for standby is prepared；
(2) PLZT powder and bismuth stearate are mixed, is mixed 20 minutes at 120 DEG C using high-speed mixer, complete powder
Last dry method coating modification；
(3) by after cladding PLZT powder and binder (mixed and formed by PEG, PVB, POM and lubricating auxiliary agent) by than
Example is uniformly mixed in mixer, prepares feeding, uses double screw extruder extruding pelletization after being crushed；
The temperature of the mixer is set as 180 DEG C, revolving speed 30r/min；Mixing twice, 10 minutes every time.
The temperature of the double screw extruder is set are as follows: and 150 DEG C, 160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, 180
DEG C, revolving speed 150rpm.
Compared with the prior art, the advantages of the present invention are as follows: method is formed compared to more conventionally employed direct pressing, is being prepared
When piezoelectric ceramics, contacts with each other between powder before being sintered, leave the space very little of crystal grain-growth for, powder is by mould side wall
Friction, there are barometric gradient inside system, crystal grain mutual extrusion in growth process, cause grain shape irregular and size not
Uniformly.Powder injection-molded rule is different, and the powder before sintering is uniformly dispersed out by adhesive, leaves after adhesive burn off
The space of enough crystal grain-growths, crystal grain are grown in a free state, shape almost spherical, and consistency is higher.This is possible to obtain
Better piezoelectric property.And the reunion between powder has then been broken in the coating modification of bismuth stearate, reduces feeding viscosity, before sintering
Phase bismuth stearate is easy to incorporate lattice, doping efficiency is than traditional oxidation in the Surface Creation nano bismuth oxide of PLZT powder
Bismuth meal last doping is high-efficient, and the amplitude for improving the piezoelectric property of PLZT is big.
Detailed description of the invention
Fig. 1 is the rheological property of different bismuth stearate dosage feedings.
Fig. 2 is different covering amount PLZT in 1280 DEG C of sintered surface SEM figures.
Fig. 3 is ferroelectric hysteresis loop of the different bismuth stearate dosage covering amount PLZT at 13kV/cm, 10Hz.
The piezoelectric constant of Fig. 4 difference bismuth stearate covering amount PLZT piezoelectric ceramics and the relationship of polarizing voltage.
Specific embodiment
Embodiment 1:
Bismuth stearate coats the powder injection-molded PP Pipe Compound and preparation method of PLZT, including PLZT powder, powder modification
Agent bismuth stearate and binder, binder are made of PEG, PVB, POM and the mixing of lubricating auxiliary agent paraffin；Feeding each component ratio
Example: PLZT powder 86.33%, polyethylene glycol (being 1:2 mixing by the mass ratio of PEG20000 and PEG1500) 7.15%, poly- second
Enol butyral (PVB) 2.15%, polyformaldehyde (POM) 2.37%, powder modifying agent bismuth stearate 0.86%, surplus are paraffin.
PLZT powder and bismuth stearate are mixed in proportion, mixed 20 minutes at 120 DEG C using high-speed mixer, is completed
Powder coating modification.
Modified powder and binder are uniformly mixed in mixer by a certain percentage, the temperature of mixer is set as
180 DEG C, revolving speed 30r/min, mixing is uniformly crushed afterwards, passes through double screw extruder extruding pelletization, temperature setting are as follows: and 150 DEG C,
160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, 180 DEG C, revolving speed 150rpm, pelletizing prepares powder injection PP Pipe Compound.
Powder injection PP Pipe Compound is injected into injection base, after will injection base be added deionized water in carry out degreasing, after degreasing
Sample prepare PLZT piezoelectric ceramics in 1280 DEG C of sinter moldings.
Embodiment 2:
Bismuth stearate coats the powder injection-molded PP Pipe Compound and preparation method of PLZT, including PLZT powder, powder modification
Agent bismuth stearate and binder, binder are made of PEG, PVB, POM and the mixing of lubricating auxiliary agent PE wax；Feeding each component ratio
Example: PLZT powder 86.33%, polyethylene glycol (being 1:3 mixing by the mass ratio of PEG20000 and PEG1500) 7.15%, poly- second
Enol butyral (PVB) 2.15%, polyformaldehyde (POM) 2.37%, powder modifying agent bismuth stearate 0.86%, surplus are PE wax.
PLZT powder and bismuth stearate are mixed in proportion, mixed 20 minutes at 120 DEG C using high-speed mixer, is completed
Powder coating modification.
Modified powder and binder are uniformly mixed in mixer by a certain percentage, the temperature of mixer is set as
180 DEG C, revolving speed 30r/min, mixing is uniformly crushed afterwards, passes through double screw extruder extruding pelletization, temperature setting are as follows: and 150 DEG C,
160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, 180 DEG C, revolving speed 150rpm, pelletizing prepares powder injection PP Pipe Compound.
Powder injection PP Pipe Compound is injected into injection base, after will injection base be added deionized water in carry out degreasing, after degreasing
Sample prepare PLZT piezoelectric ceramics in 1280 DEG C of sinter moldings.
Embodiment 3:
Bismuth stearate coats the powder injection-molded PP Pipe Compound and preparation method of PLZT, including PLZT powder, powder modification
Agent bismuth stearate and binder, binder are mixed by PEG, PVB, POM and lubricating auxiliary agent (paraffin and PE wax mass ratio 1:1 mixing)
It is combined into；Feeding each component ratio: (mass ratio by PEG20000 and PEG1500 is for PLZT powder 86.33%, polyethylene glycol
1:2 mixing) 7.15%, polyvinyl butyral (PVB) 2.58%, polyformaldehyde (POM) 2.02%, powder modifying agent bismuth stearate
3.81%, surplus is that paraffin and PE wax mass ratio 1:1 are mixed.
PLZT powder and bismuth stearate are mixed in proportion, mixed 20 minutes at 120 DEG C using high-speed mixer, is completed
Powder coating modification.
By after coating modification powder and binder by a certain percentage in mixer be uniformly mixed, the temperature of mixer is set
It is set to 180 DEG C, revolving speed 30r/min, mixing is uniformly crushed afterwards, passes through double screw extruder extruding pelletization, temperature setting are as follows:
150 DEG C, 160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, 180 DEG C, revolving speed 150rpm, pelletizing prepares powder injection PP Pipe Compound.
Powder injection PP Pipe Compound is injected into injection base, after will injection base be added deionized water in carry out degreasing, after degreasing
Sample prepare PLZT piezoelectric ceramics in 1280 DEG C of sinter moldings.
Comparative example 1:
Bismuth stearate coats the powder injection-molded PP Pipe Compound and preparation method of PLZT, including PLZT powder, powder modification
Agent bismuth stearate and binder, binder are mixed by PEG, PVB, POM and lubricating auxiliary agent (paraffin and PE wax mass ratio 1:1 mixing)
It is combined into；Feeding each component ratio: (mass ratio by PEG20000 and PEG1500 is for PLZT powder 86.33%, polyethylene glycol
1:2 mixing) 7.15%, polyvinyl butyral (PVB) 2.58%, polyformaldehyde (POM) 2.02%, (bismuth contains bismuth oxide 1.74%
Measure same as Example 3), surplus be that paraffin and PE wax mass ratio 1:1 are mixed.
Modified powder and binder are uniformly mixed in mixer by a certain percentage, the temperature of mixer is set as
180 DEG C, revolving speed 30r/min, mixing is uniformly crushed afterwards, passes through double screw extruder extruding pelletization, temperature setting are as follows: and 150 DEG C,
160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, 180 DEG C, revolving speed 150rpm, pelletizing prepares powder injection PP Pipe Compound.
Powder injection PP Pipe Compound is injected into injection base, after will injection base be added deionized water in carry out degreasing, after degreasing
Sample prepare PLZT piezoelectric ceramics in 1280 DEG C of sinter moldings.
Comparative example 2:
The powder injection-molded preparation method for material special of PLZT, including PLZT powder and binder, binder be by PEG,
PVB, POM and lubricating auxiliary agent paraffin mixing composition；Feeding each component ratio: PLZT powder 87.19%, polyethylene glycol (by
The mass ratio of PEG20000 and PEG1500 is 1:2 mixing) 7.11%, polyvinyl butyral (PVB) 2.37%, polyformaldehyde
(POM) 2.37%, surplus is paraffin.
Powder and binder are uniformly mixed in mixer by a certain percentage, the temperature of mixer is set as 180 DEG C, turns
Speed is 30r/min, and mixing is uniformly crushed afterwards, passes through double screw extruder extruding pelletization, temperature setting are as follows: 150 DEG C, 160 DEG C,
170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, 180 DEG C, revolving speed 150rpm, pelletizing prepares powder injection PP Pipe Compound.
Powder injection PP Pipe Compound is injected into injection base, after will injection base be added deionized water in carry out degreasing, after degreasing
Sample prepare PLZT piezoelectric ceramics in 1280 DEG C of sinter moldings.
Comparative example 3:
PLZT piezoelectric ceramics is prepared using dry powder pressing, the PLZT powder each group distribution ratio of selection is: Pb0.91La0.06
(Zr0.58Ti0.42)0.975Nb0.02O3, wherein Pb3O4For 64.43%, La2O3For 3.03%, ZrO2For 21.59%, TiO2For
10.13% and Nb2O5It is 0.82%.1280 DEG C of sintering temperature, sintering time 90min.
Embodiment 1-3, comparative example 1-3 are subjected to following performance detection comparison, testing result such as table 1
Table 1
Claims (8)
1. a kind of powder injection-molded PP Pipe Compound of bismuth stearate cladding lead lanthanum zirconate titanate；It is characterized in that, the powder includes:
Lead lanthanum zirconate titanate (PLZT) powder, bismuth stearate and binder；
Binder is made of PEG, PVB, POM and lubricating auxiliary agent mixing；
The mass percent of the injection moulding PP Pipe Compound each component is as follows: PLZT powder 86.87~88.99%, polyethylene glycol
(PEG) 6.01~7.88%, polyvinyl butyral (PVB) 2.00~2.62%, polyformaldehyde (POM) 2.00~2.62%, powder
Modifies dose 0.50~4.00%, surplus be lubricating auxiliary agent.
2. the powder injection-molded PP Pipe Compound of bismuth stearate cladding lead lanthanum zirconate titanate according to claim 1, feature exist
In selected PLZT powder each group distribution ratio is: Pb0.91La0.06(Zr0.58Ti0.42)0.975Nb0.02O3, wherein Pb3O4For
64.43%, La2O3For 3.03%, ZrO2For 21.59%, TiO2For 10.13% and Nb2O5It is 0.82%.
3. the powder injection-molded PP Pipe Compound of bismuth stearate cladding lead lanthanum zirconate titanate according to claim 1, feature exist
In the powder modifier is bismuth stearate, and preparation method is prepared using one-step method, i.e., heats stearic acid molten
Bi is put into after melting2O3, by stearic acid and Bi2O3Molar ratio 1:(0.47-0.49) it feeds intake, add the glacial acetic acid of stearic acid dosage 3%
As catalyst, 2% isopropanol reacts two hours at 130 DEG C as foam in hibitors.
4. the powder injection-molded PP Pipe Compound of bismuth stearate cladding lead lanthanum zirconate titanate according to claim 1, feature exist
In the PEG is the PEG mixture of different molecular weight, wherein wherein PEG20000 and PEG1500 1:(2-3 in mass ratio) group
At low molecular weight PEG1500 is used for quick water degreasing, and high molecular weight PEGs 20000 are for obtaining higher powder loading.
5. the powder injection-molded PP Pipe Compound of bismuth stearate cladding lead lanthanum zirconate titanate according to claim 1, feature exist
In the lubricating auxiliary agent is one of paraffin and polyethylene wax or mixture.
6. a kind of bismuth stearate cladding lead lanthanum zirconate titanate according to claim 1-5 is powder injection-molded dedicated
The preparation method of material, which is characterized in that specific feeding the preparation method is as follows:
(1) preparation of PLZT powder: with Pb3O4、La2O3、ZrO2、TiO2And Nb2O5To prepare raw material, purity is all larger than 99%, is
Holding stoichiometry, all oxides are sufficiently dry before weighing, and raw material is after ball milling mixing is uniform in 850 DEG C of calcining 2h
PLZT powder, ball milling sieving for standby is prepared；
(2) PLZT powder and powder modifier are mixed, is mixed 20 minutes at 120 DEG C using high-speed mixer, complete powder
Dry method coating modification；
(3) by after cladding PLZT powder and binder in proportion in mixer be uniformly mixed, mixing uniformly afterwards be crushed use
Double screw extruder extruding pelletization prepares powder injection-molded PP Pipe Compound.
7. the preparation side of the powder injection-molded PP Pipe Compound of bismuth stearate cladding lead lanthanum zirconate titanate according to claim 6
Method, which is characterized in that the temperature of step (3) mixer is set as 180 DEG C, revolving speed 30r/min；Mixing twice, every time
10 minutes.
8. the preparation side of the powder injection-molded PP Pipe Compound of bismuth stearate cladding lead lanthanum zirconate titanate according to claim 6
Method, which is characterized in that the temperature of step (3) double screw extruder is set are as follows: 150 DEG C, 160 DEG C, 170 DEG C, 175 DEG C, 180
DEG C, 180 DEG C, 180 DEG C, revolving speed 150rpm.
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| CN117326866A (en) * | 2023-12-01 | 2024-01-02 | 山东利恩斯智能科技有限公司 | Cerium-manganese co-doped lead zirconate titanate-based piezoelectric ceramic material and preparation method thereof |
| CN117326866B (en) * | 2023-12-01 | 2024-02-23 | 山东利恩斯智能科技有限公司 | Cerium-manganese co-doped lead zirconate titanate-based piezoelectric ceramic material and preparation method thereof |
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