CN110204334A - A kind of high-compactness Zirconium oxide powder injection moulding PP Pipe Compound and preparation method thereof - Google Patents
A kind of high-compactness Zirconium oxide powder injection moulding PP Pipe Compound and preparation method thereof Download PDFInfo
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- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The present invention relates to a kind of high-compactness Zirconium oxide powder injection moulding PP Pipe Compounds and preparation method thereof, including following component raw material: Zirconium oxide powder 86.87~88.99%, polyethylene glycol 6.01~7.88%, polyvinyl butyral 2.00~2.62%, polyformaldehyde 2.00~2.62%, yttrium stearate 0.50~3.60%, surplus are lubricating auxiliary agent, first Zirconium oxide powder is surface-treated using yttrium stearate, then it is mixed in mixer with binder, broken rear extruding pelletization is simultaneously injection moulded, and sinters porcelain into after completing degreasing in deionized water.The present invention is by yttrium stearate to the processing of Zirconium oxide powder cladding, reduce feeding viscosity, finished product compactness greatly improves after sintering, solve agglomeration traits of the powdered zirconium oxide end in process of injection molding, and nano yttrium oxide particle is generated by sintering, it is easier to diffuse into lattice, doping efficiency greatly improves, so that ceramic dense degree improves.
Description
Technical field
The present invention relates to powder injection molding technology more particularly to a kind of injection moulding of high-compactness Zirconium oxide powder are dedicated
The preparation method of material.
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 zirconia ceramics, yttrium is a kind of common ceramic doped chemical, for proposing zirconium oxide consistency, drop
Sintering temperature and low.Yttrium stearate coating modification Zirconium oxide powder is used to this research and innovation, using water-soluble resin macromolecular
Binder has prepared low viscosity, the injection PP Pipe Compound of good dispersion, and PP Pipe Compound is prepared through injection moulding, water degreasing, sintering
High-compactness zirconia ceramics.This research uses yttrium stearate coating modification Zirconium oxide powder, not only solves powdered zirconium oxide
Agglomeration traits of the end in process of injection molding, and yttrium stearate sintering process can zirconium surface generate it is nano oxidized
Yttrium, nano yttrium oxide are uniformly dispersed, easily enter zirconia crystal lattice, play the role of doping vario-property, and the powder that compares directly adds
Add, yttrium stearate doping efficiency and implant uniformity have been greatly improved.
Summary of the invention
The technical problem to be solved by the present invention is providing, a kind of injection moulding of high-compactness Zirconium oxide powder is dedicated and its system
Preparation Method prepares the PP Pipe Compound of low viscosity, high-intensitive green body using stearic acid yttrium coating modification, and improves former zirconium oxide pottery
The consistency of porcelain, makes it have more the market competitiveness.
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 high
Consistency Zirconium oxide powder is injection moulded the preparation method of PP Pipe Compound, and it includes following:
Zirconium oxide powder, yttrium stearate and binder, binder are made of PEG, PVB, POM and lubricating auxiliary agent mixing；
The mass percent of above-mentioned each component is as follows: Zirconium oxide 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%, yttrium stearate 0.50~
3.60%, surplus is lubricating auxiliary agent.
The mixing of one or more of the Zirconium oxide powder that the Zirconium oxide powder is 1-2 μm and 5-10 μm of particle size range
Object.
The modifying agent yttrium stearate is prepared using one-step method, i.e., will put into and aoxidize after stearic acid heating melting
Yttrium (1:0.46-0.48 feeds intake in molar ratio) adds the glacial acetic acid of stearic acid dosage 3% as catalyst, stearic acid dosage 2%
Isopropanol as foam in hibitors, reacted two hours at 150 DEG C, nitrogen protection.
The PEG is the PEG mixture of high low molecular weight collocation, i.e. PEG1500 and PEG20000 are mixed for 2:1 in mass ratio
It closes；Low molecular weight PEG1500 is used for quick water degreasing, and degreasing efficiency can improve, and high molecular weight PEGs 20000 are higher for obtaining
Powder loading.
Specific feeding the preparation method is as follows:
(1) Zirconium oxide powder and yttrium stearate are mixed in a certain ratio, using high-speed mixer at 150 DEG C
10Min completes powder coating modification；
(2) by after cladding Zirconium oxide powder and binder in proportion in mixer be uniformly mixed, prepare feeding, be crushed
Single screw extrusion machine extruding pelletization is used afterwards, prepares high-compactness Zirconium oxide powder injection moulding PP Pipe Compound；
The temperature of mixer is set as 180 DEG C, revolving speed 30r/min；Mixing twice, 10 minutes every time.
The temperature of single screw extrusion machine is set are as follows: and 150 DEG C, 160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, revolving speed 150-
200rpm。
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.And powder injection-molded rule is different, the powder before sintering is uniformly dispersed out by adhesive, is left after adhesive removing
The space of enough crystal grain-growths, crystal grain are grown in a free state, shape almost spherical, and consistency is higher.Meanwhile the application
Using the coating modification Zirconium powder of yttrium stearate, the reunion between powder is effectively broken, has reduced feeding viscosity, has been sintered
Later period generates nano yttrium oxide in zirconium surface, and nano yttrium oxide is uniformly dispersed, and easily incorporates lattice, improves yttrium oxide
The uniformity and doping efficiency of doped zirconia, so that ceramic dense degree and performance greatly improve.
Detailed description of the invention
Fig. 1 is the mechanism schematic diagram that zirconium oxide adulterates in situ；
Fig. 2 is the SEM figure of the zirconia ceramics of the powder injection-molded preparation of embodiment 3.
Specific embodiment
Embodiment 1:
High-compactness Zirconium oxide powder is injection moulded PP Pipe Compound, is made of Zirconium oxide powder and binder, wherein bonding
Agent is made of PEG, PVB, POM and the mixing of lubricating auxiliary agent PE wax.
Feeding each component ratio: Zirconium oxide powder (1-2 μm of partial size) 87.19%, polyethylene glycol (PEG1500 and
PEG20000 is 2:1 mixing in mass ratio) 7.11%, polyvinyl butyral (PVB) 2.37%, polyformaldehyde (POM) 2.37%,
Yttrium stearate 1%, surplus are PE wax.
Powder Oxidation zirconium and yttrium stearate are used by a certain percentage in high-speed mixer and mix 10min at 150 DEG C, it is complete
At coating modification.
The zirconium oxide and binder of coating modification are uniformly mixed in mixer by a certain percentage, the temperature setting of mixer
It is 180 DEG C, revolving speed 30r/min, twice, 10 minutes every time, mixing was uniformly crushed afterwards for mixing, was squeezed out by single screw extrusion machine
It is granulated, temperature setting are as follows: 150 DEG C, 160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, revolving speed 150rpm, pelletizing prepares powder
Inject 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 zirconia ceramics in 1500 DEG C of sinter moldings.
Embodiment 2:
High-compactness Zirconium oxide powder is injection moulded PP Pipe Compound, is made of Zirconium oxide powder and binder, wherein bonding
Agent is made of PEG, PVB, POM and the mixing of lubricating auxiliary agent paraffin.
Feeding each component ratio: Zirconium oxide powder (5-10 μm of partial size) 87.19%, polyethylene glycol (PEG1500 and
PEG20000 is 2:1 mixing in mass ratio) 7.11%, polyvinyl butyral (PVB) 2.12%, polyformaldehyde (POM) 2.48%,
Yttrium stearate 2%, surplus are paraffin.
Powder Oxidation zirconium and yttrium stearate are used by a certain percentage in high-speed mixer and mix 10min at 150 DEG C, it is complete
At coating modification.
The zirconium oxide and binder of coating modification are uniformly mixed in mixer by a certain percentage, the temperature setting of mixer
It is 180 DEG C, revolving speed 30r/min, twice, 10 minutes every time, mixing was uniformly crushed afterwards for mixing, was squeezed out by single screw extrusion machine
It is granulated, temperature setting are as follows: 150 DEG C, 160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, revolving speed 200rpm, pelletizing prepares powder
Inject 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 zirconia ceramics in 1500 DEG C of sinter moldings.
Embodiment 3:
High-compactness Zirconium oxide powder is injection moulded PP Pipe Compound, is made of Zirconium oxide powder and binder, wherein bonding
Agent is made of PEG, PVB, POM and lubricating auxiliary agent (the mass ratio 1:1 of PE wax and paraffin mixing) mixing.
Feeding each component ratio: Zirconium oxide powder (1-2 μm and 5-10 μm mixing of 1:1 in mass ratio of partial size) 87.19% gathers
It is ethylene glycol (PEG1500 and PEG20000 are 2:1 mixing in mass ratio) 7.11%, polyvinyl butyral (PVB) 2.37%, poly-
Formaldehyde (POM) 2.37%, yttrium stearate 3%, surplus are the mass ratio 1:1 mixing of PE wax and paraffin.
Powder Oxidation zirconium and yttrium stearate are used by a certain percentage in high-speed mixer and mix 10min at 150 DEG C, it is complete
At coating modification.
The zirconium oxide and binder of coating modification are uniformly mixed in mixer by a certain percentage, the temperature setting of mixer
It is 180 DEG C, revolving speed 30r/min, twice, mixing in 10 minutes is uniformly crushed afterwards every time for mixing, is squeezed out by single screw extrusion machine
It is granulated, temperature setting are as follows: 150 DEG C, 160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, revolving speed 150rpm, pelletizing prepares powder
Inject 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 zirconia ceramics in 1500 DEG C of sinter moldings.
Comparative example 1: zirconia ceramics, sintering temperature 1500 are prepared using Zirconium oxide powder (1-2 μm of partial size) direct pressing
DEG C, sintering time 90min.
Comparative example 2:
Zirconium oxide powder be injection moulded PP Pipe Compound, be made of Zirconium oxide powder and binder, wherein binder by PEG,
PVB, POM and lubricating auxiliary agent mixing composition.
Feeding each component ratio: Zirconium oxide powder (1-2 μm of partial size) 87.19%, polyethylene glycol (PEG1500 and
PEG20000 is 2:1 mixing in mass ratio) 7.11%, polyvinyl butyral (PVB) 2.37%, polyformaldehyde (POM) 2.37%,
Surplus is PE wax.
Powder Oxidation zirconium 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, and mixing twice, 10 minutes every time, is made by single screw extrusion machine extrusion
Grain, temperature setting are as follows: 150 DEG C, 160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, revolving speed 180rpm, pelletizing prepares powder note
Penetrate 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 zirconia ceramics in 1500 DEG C of sinter moldings.
Comparative example 3:
Zirconium oxide powder be injection moulded PP Pipe Compound, be made of Zirconium oxide powder and binder, wherein binder by PEG,
PVB, POM and lubricating auxiliary agent mixing composition.
Feeding each component ratio: Zirconium oxide powder (1-2 μm and 5-10 μm mixing of 1:1 in mass ratio of partial size) 87.19% gathers
It is ethylene glycol (PEG1500 and PEG20000 are 2:1 mixing in mass ratio) 7.11%, polyvinyl butyral (PVB) 2.37%, poly-
Formaldehyde (POM) 2.37%, yttrium oxide 0.8%, surplus are the mass ratio 1:1 mixing of PE wax and paraffin.
Powder Oxidation zirconium, yttrium oxide, binder are uniformly mixed in mixer by a certain percentage, the temperature of mixer is set
It is set to 180 DEG C, revolving speed 30r/min, twice, 10 minutes every time, mixing was uniformly crushed afterwards for mixing, was squeezed by single screw extrusion machine
It is granulated out, temperature setting are as follows: 150 DEG C, 160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, revolving speed 150rpm, pelletizing prepares powder
End 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 zirconia ceramics in 1500 DEG C of sinter moldings.
Performance test comparison:
Claims (8)
1. a kind of high-compactness Zirconium oxide powder is injection moulded PP Pipe Compound；It is characterised by comprising: Zirconium oxide powder, stearic acid
Yttrium and binder；
It is described to be made of binder PEG, PVB, POM and lubricating auxiliary agent mixing；
The mass percent for being injection moulded each component of PP Pipe Compound is as follows: Zirconium oxide powder 86.87~88.99%, polyethylene glycol
6.01~7.88%, polyvinyl butyral (PVB) 2.00~2.62%, polyformaldehyde (POM) 2.00~2.62%, yttrium stearate
0.50~3.60%, surplus is lubricating auxiliary agent.
2. high-compactness Zirconium oxide powder according to claim 1 is injection moulded PP Pipe Compound, which is characterized in that the oxygen
Change one or more of the Zirconium oxide powder that zirconium powder is 1-2 μm and 5-10 μm of particle size range mixture.
3. high-compactness Zirconium oxide powder according to claim 1 is injection moulded PP Pipe Compound, which is characterized in that described is hard
Resin acid yttrium modifying agent is prepared using one-step method, i.e., will put into yttrium oxide after stearic acid heating melting, in molar ratio 1:
(0.46-0.48) feeds intake, and adds the glacial acetic acid of stearic acid dosage 3% as catalyst, the isopropanol conduct of stearic acid dosage 2%
Foam in hibitors reacts two hours, nitrogen protection at 150 DEG C.
4. high-compactness Zirconium oxide powder according to claim 1 is injection moulded PP Pipe Compound, which is characterized in that the PEG
For the PEG mixture of high low molecular weight collocation, i.e. PEG1500 and PEG20000 are 2:1 mixing in mass ratio；Low molecular weight
PEG1500 is used for quick water degreasing, and high molecular weight PEGs 20000 are for obtaining higher powder loading.
5. high-compactness Zirconium oxide powder according to claim 1 is injection moulded PP Pipe Compound, which is characterized in that the lubrication
Auxiliary agent is one or more of mixing of paraffin and PE wax.
6. a kind of preparation side of high-compactness Zirconium oxide powder injection moulding PP Pipe Compound according to claim 1-5
Method, which is characterized in that specific feeding the preparation method is as follows:
(1) Zirconium oxide powder and yttrium stearate are mixed in a certain ratio, 10min, completion at 150 DEG C using high-speed mixer
Powder coating modification；
(2) by after coating modification Zirconium oxide powder and binder in proportion in mixer be uniformly mixed, prepare feeding, be crushed
Single screw extrusion machine extruding pelletization is used afterwards, prepares high-compactness Zirconium oxide powder injection moulding PP Pipe Compound.
7. the preparation method of high-compactness Zirconium oxide powder injection moulding PP Pipe Compound according to claim 6, feature exist
In the temperature of step (2) mixer is set as 180 DEG C, revolving speed 30r/min；Mixing twice, 10 minutes every time.
8. the preparation method of high-compactness Zirconium oxide powder injection moulding PP Pipe Compound according to claim 6, feature exist
In the temperature setting of step (2) single screw extrusion machine are as follows: 150 DEG C, 160 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 180 DEG C, turn
Fast 150-200rpm.
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