CN110204334B - Special material for high-density zirconium oxide powder injection molding and preparation method thereof - Google Patents
Special material for high-density zirconium oxide powder injection molding and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a special material for high-density zirconia powder injection molding and a preparation method thereof, and the special material comprises the following raw materials: 86.87-88.99% of zirconia powder, 6.01-7.88% of polyethylene glycol, 2.00-2.62% of polyvinyl butyral, 2.00-2.62% of polyformaldehyde, 0.50-3.60% of yttrium stearate and the balance of a lubricating aid, wherein the zirconia powder is subjected to surface treatment by adopting the yttrium stearate, then is mixed with a binder in an internal mixer, is crushed, is extruded for granulation and injection molding, is degreased in deionized water and is sintered into a ceramic. According to the invention, the yttrium stearate is used for coating the zirconia powder, so that the feeding viscosity is reduced, the compactness of the sintered finished product is greatly improved, the problem of agglomeration of the zirconia fine powder in the injection molding process is solved, the nano yttrium oxide particles are generated by sintering, the nano yttrium oxide particles are easy to diffuse into crystal lattices, the doping efficiency is greatly improved, and the ceramic compactness is improved.
Description
Technical Field
The invention relates to a powder injection molding technology, in particular to a preparation method of a special material for high-density zirconia powder injection molding.
Background
Powder injection molding is a new near-net shape molding technology developed on the basis of plastic injection molding and powder metallurgy. The method comprises the following steps of taking a mixture of metal or inorganic powder and a binder as a feed, injecting the feed with a flowing state into a mold cavity by an injection machine under certain pressure, temperature and speed, cooling to obtain an injection green compact, and then degreasing, sintering and simply performing subsequent processing to obtain a finished product. The product has good surface quality, high density and high precision, and is easy to realize automatic production.
In order to solve the problems of low solid content, easy agglomeration and the like of fine powder in injection molding, various surfactants are used for pretreating the powder in the most common method. Surfactants can be broadly classified into two categories: one is fatty acid (SA, OA, HSA) which is adsorbed on the surface of the ceramic powder through Lewis acid-base reaction hydrogen bonds; another class is coupling agents (silanes, titanates) which are covalently bonded to the ceramic powder. They all act as a bridge between the molten polymer and the ceramic powder, improving the dispersion of the ceramic powder in the binder, thereby increasing the compatibility between the binder components and reducing the viscosity.
For zirconia ceramics, yttrium is a common ceramic doping element used for increasing the compactness of zirconia and reducing the sintering temperature. According to the research, yttrium stearate is innovatively used for coating modified zirconia powder, a water-soluble resin macromolecular binder is adopted to prepare the special injection material with low viscosity and good dispersibility, and the special injection material is subjected to injection molding, water degreasing and sintering to prepare the high-density zirconia ceramic. According to the research, yttrium stearate is used for coating the modified zirconia powder, the problem of agglomeration of the zirconia fine powder in the injection molding process is solved, nanometer yttrium oxide can be generated on the surface of zirconia in the sintering process of the yttrium stearate, the nanometer yttrium oxide is uniformly dispersed and can easily enter zirconia lattices to play a role in doping modification, and compared with the direct addition of powder, the yttrium stearate doping efficiency and the doping uniformity are greatly improved.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method is characterized in that yttrium stearate is used for coating and modifying to prepare the special material for the low-viscosity and high-strength green body, and the density of the original zirconia ceramic is improved, so that the zirconia ceramic has higher market competitiveness.
The technical problem to be solved by the invention is realized by adopting the following technical scheme. The preparation method of the special material for the high-density zirconia powder injection molding provided by the invention comprises the following steps:
zirconium oxide powder, yttrium stearate and a binder, wherein the binder is formed by mixing PEG, PVB, POM and a lubricating additive; the mass percentages of the components are as follows: 86.87-88.99% of zirconia powder, 6.01-7.88% of polyethylene glycol (PEG), 2.00-2.62% of polyvinyl butyral (PVB), 2.00-2.62% of Polyformaldehyde (POM), 0.50-3.60% of yttrium stearate and the balance of a lubricating assistant.
The zirconia powder is one or a mixture of zirconia powder with the particle size range of 1-2 μm and zirconia powder with the particle size range of 5-10 μm.
The modifier yttrium stearate is prepared by a one-step method, namely, yttrium oxide (fed according to the molar ratio of 1: 0.46-0.48) is added after stearic acid is heated and melted, glacial acetic acid with the stearic acid amount being 3% is added as a catalyst, isopropanol with the stearic acid amount being 2% is added as a foam inhibitor, and the mixture reacts for two hours at 150 ℃ under the protection of nitrogen.
The PEG is a PEG mixture with high and low molecular weight matching, namely PEG1500 and PEG20000 are mixed according to the mass ratio of 2: 1; the low molecular weight PEG1500 is used for fast water degreasing, the degreasing efficiency will be improved, and the high molecular weight PEG20000 is used to obtain higher powder loading.
The specific feed preparation method is as follows:
(1) mixing zirconium oxide powder and yttrium stearate according to a certain proportion, and using a high-speed mixer to complete powder coating modification at the temperature of 150 ℃ for 10 Min;
(2) uniformly mixing the coated zirconia powder and a binder in an internal mixer according to a proportion, preparing a feed, crushing, and then extruding and granulating by using a single-screw extruder to prepare a high-density zirconia powder injection molding special material;
the temperature of the internal mixer is set to be 180 ℃, and the rotating speed is 30 r/min; banburying twice for 10 minutes each time.
The temperature of the single screw extruder was set to: 150 ℃, 160 ℃, 170 ℃, 175 ℃, 180 ℃, 180 ℃, and the rotation speed of 150 ℃ and 200 rpm.
Compared with the prior art, the invention has the advantages that: compared with the traditional direct pressing and forming method, when piezoelectric ceramics are prepared, the powder is in mutual contact before sintering, the space reserved for grain growth is very small, the powder is rubbed by the side wall of the mold, the pressure gradient exists inside the system, and the grains are mutually extruded in the growing process, so that the grains are irregular in shape and uneven in size. The powder injection molding method is different, the powder before sintering is uniformly dispersed by the adhesive, a space enough for grain growth is left after the adhesive is removed, the grains grow in a free state, the shape is similar to a sphere, and the density is higher. Meanwhile, the yttrium stearate is coated and modified on the zirconia powder, so that agglomeration among the powder is effectively broken, the feeding viscosity is reduced, the nano yttrium oxide is generated on the surface of the zirconia in the later sintering period, the nano yttrium oxide is uniformly dispersed and is easily fused into crystal lattices, the uniformity and the doping efficiency of yttrium oxide doped zirconia are improved, and the density and the performance of the ceramic are greatly improved.
Drawings
FIG. 1 is a schematic diagram of the mechanism of in-situ doping of zirconia;
FIG. 2 is an SEM image of a zirconia ceramic prepared by powder injection molding of example 3.
Detailed Description
Example 1:
the special material for high-density zirconia powder injection molding consists of zirconia powder and a binder, wherein the binder is formed by mixing PEG, PVB, POM and a lubricating additive PE wax.
The feed comprises the following components in proportion: 87.19% of zirconium oxide powder (with the particle size of 1-2 μm), 7.11% of polyethylene glycol (PEG1500 and PEG20000 are mixed according to the mass ratio of 2: 1), 2.37% of polyvinyl butyral (PVB), 2.37% of Polyformaldehyde (POM), 1% of yttrium stearate and the balance of PE wax.
And mixing the powder zirconium oxide and the yttrium stearate in a high-speed mixer according to a certain proportion at 150 ℃ for 10min to finish coating modification.
Uniformly mixing the coated and modified zirconia and a binder in an internal mixer according to a certain proportion, setting the temperature of the internal mixer to be 180 ℃, setting the rotating speed to be 30r/min, internally mixing twice for 10 minutes each time, crushing after uniform internal mixing, extruding and granulating through a single-screw extruder, and setting the temperature to be: cutting the mixture into particles at 150 ℃, 160 ℃, 170 ℃, 175 ℃, 180 ℃ and the rotation speed of 150rpm to prepare the special powder injection material.
Injecting the special powder injection material into an injection blank, adding the injection blank into deionized water for degreasing, and sintering and molding the degreased sample at 1500 ℃ to prepare the zirconia ceramic.
Example 2:
the special material for high-density zirconia powder injection molding consists of zirconia powder and a binder, wherein the binder is formed by mixing PEG, PVB, POM and a lubricating additive paraffin.
The feed comprises the following components in proportion: 87.19 percent of zirconium oxide powder (with the particle size of 5-10 mu m), 7.11 percent of polyethylene glycol (PEG1500 and PEG20000 are mixed according to the mass ratio of 2: 1), 2.12 percent of polyvinyl butyral (PVB), 2.48 percent of Polyformaldehyde (POM), 2 percent of yttrium stearate and the balance of paraffin.
And mixing the powder zirconium oxide and the yttrium stearate in a high-speed mixer according to a certain proportion at 150 ℃ for 10min to finish coating modification.
Uniformly mixing the coated and modified zirconia and a binder in an internal mixer according to a certain proportion, setting the temperature of the internal mixer to be 180 ℃, setting the rotating speed to be 30r/min, internally mixing twice for 10 minutes each time, crushing after uniform internal mixing, extruding and granulating through a single-screw extruder, and setting the temperature to be: cutting the mixture into particles at 150 ℃, 160 ℃, 170 ℃, 175 ℃, 180 ℃ and the rotation speed of 200rpm to prepare the special powder injection material.
Injecting the special powder injection material into an injection blank, adding the injection blank into deionized water for degreasing, and sintering and molding the degreased sample at 1500 ℃ to prepare the zirconia ceramic.
Example 3:
the special material for high-density zirconia powder injection molding consists of zirconia powder and a binder, wherein the binder is formed by mixing PEG, PVB, POM and a lubricating additive (the mass ratio of PE wax to paraffin wax is 1: 1).
The feed comprises the following components in proportion: 87.19% of zirconia powder (particle size of 1-2 μm and 5-10 μm mixed at a mass ratio of 1: 1), 7.11% of polyethylene glycol (PEG1500 and PEG20000 mixed at a mass ratio of 2: 1), 2.37% of polyvinyl butyral (PVB), 2.37% of Polyoxymethylene (POM), 3% of yttrium stearate, and the balance of PE wax and paraffin wax at a mass ratio of 1: 1 and mixing.
And mixing the powder zirconium oxide and the yttrium stearate in a high-speed mixer according to a certain proportion at 150 ℃ for 10min to finish coating modification.
Uniformly mixing the coated and modified zirconia and a binder in an internal mixer according to a certain proportion, setting the temperature of the internal mixer to be 180 ℃, setting the rotating speed to be 30r/min, internally mixing twice, crushing after uniformly mixing for 10 minutes each time, and extruding and granulating through a single-screw extruder, wherein the temperature is set as follows: cutting the mixture into particles at 150 ℃, 160 ℃, 170 ℃, 175 ℃, 180 ℃ and the rotation speed of 150rpm to prepare the special powder injection material.
Injecting the special powder injection material into an injection blank, adding the injection blank into deionized water for degreasing, and sintering and molding the degreased sample at 1500 ℃ to prepare the zirconia ceramic.
Comparative example 1: zirconia powder (with the grain diameter of 1-2 mu m) is directly pressed to prepare the zirconia ceramics, the sintering temperature is 1500 ℃, and the sintering time is 90 min.
Comparative example 2:
the special material for zirconia powder injection molding consists of zirconia powder and a binder, wherein the binder is formed by mixing PEG, PVB, POM and a lubricating additive.
The feed comprises the following components in proportion: 87.19% of zirconium oxide powder (with the particle size of 1-2 μm), 7.11% of polyethylene glycol (PEG1500 and PEG20000 are mixed according to the mass ratio of 2: 1), 2.37% of polyvinyl butyral (PVB), 2.37% of Polyformaldehyde (POM) and the balance of PE wax.
Uniformly mixing powder zirconia and a binder in an internal mixer according to a certain proportion, setting the temperature of the internal mixer to be 180 ℃, setting the rotating speed to be 30r/min, crushing after uniform internal mixing, carrying out internal mixing twice for 10 minutes each time, extruding and granulating through a single-screw extruder, and setting the temperature to be: cutting the mixture into particles at 150 ℃, 160 ℃, 170 ℃, 175 ℃, 180 ℃, 180 ℃ and 180rpm to prepare the special powder injection material.
Injecting the special powder injection material into an injection blank, adding the injection blank into deionized water for degreasing, and sintering and molding the degreased sample at 1500 ℃ to prepare the zirconia ceramic.
Comparative example 3:
the special material for zirconia powder injection molding consists of zirconia powder and a binder, wherein the binder is formed by mixing PEG, PVB, POM and a lubricating additive.
The feed comprises the following components in proportion: 87.19% of zirconia powder (particle size of 1-2 μm and 5-10 μm mixed at a mass ratio of 1: 1), 7.11% of polyethylene glycol (PEG1500 and PEG20000 mixed at a mass ratio of 2: 1), 2.37% of polyvinyl butyral (PVB), 2.37% of Polyoxymethylene (POM), 0.8% of yttria, and the balance of PE wax and paraffin wax at a mass ratio of 1: 1 and mixing.
Uniformly mixing powder zirconium oxide, yttrium oxide and a binder in an internal mixer according to a certain proportion, setting the temperature of the internal mixer to be 180 ℃, setting the rotating speed to be 30r/min, internally mixing twice, each time for 10 minutes, crushing after uniform internal mixing, extruding and granulating through a single-screw extruder, and setting the temperature to be: cutting the mixture into particles at 150 ℃, 160 ℃, 170 ℃, 175 ℃, 180 ℃ and the rotation speed of 150rpm to prepare the special powder injection material.
Injecting the special powder injection material into an injection blank, adding the injection blank into deionized water for degreasing, and sintering and molding the degreased sample at 1500 ℃ to prepare the zirconia ceramic.
And (3) performance test comparison:
Claims (7)
1. a special material for high-density zirconia powder injection molding; it is characterized by comprising: zirconium oxide powder, yttrium stearate and a binder;
the adhesive is formed by mixing PEG, PVB, POM and a lubricating additive;
the mass percentage of each component of the injection molding special material is as follows: 86.87-88.99% of zirconia powder, 6.01-7.88% of polyethylene glycol, 2.00-2.62% of polyvinyl butyral (PVB), 2.00-2.62% of Polyformaldehyde (POM), 0.50-3.60% of yttrium stearate and the balance of a lubricating assistant;
the yttrium stearate modifier is prepared by a one-step method, namely heating and melting stearic acid, and then adding yttrium oxide into the heated and melted stearic acid, wherein the molar ratio of yttrium oxide to yttrium oxide is 1: (0.46-0.48) feeding, adding glacial acetic acid with the stearic acid amount being 3% as a catalyst, adding isopropanol with the stearic acid amount being 2% as a foam inhibitor, reacting for two hours at 150 ℃, and protecting with nitrogen.
2. The special material for injection molding of high-density zirconia powder according to claim 1, wherein the zirconia powder is one or a mixture of zirconia powders with the particle size ranges of 1-2 μm and 5-10 μm.
3. The special material for injection molding of high-density zirconia powder according to claim 1, wherein the PEG is a mixture of PEGs with high and low molecular weights, i.e. PEG1500 and PEG20000 are mixed in a mass ratio of 2: 1; the low molecular weight PEG1500 is used for fast water degreasing and the high molecular weight PEG20000 is used to obtain higher powder loading.
4. The special material for high-density zirconia powder injection molding according to claim 1, wherein the lubricating additive is one or a mixture of paraffin wax and PE wax.
5. The preparation method of the special material for high-density zirconia powder injection molding according to any one of claims 1 to 4, characterized in that the specific feeding material preparation method is as follows:
(1) mixing zirconium oxide powder and yttrium stearate according to a certain proportion, and using a high-speed mixer for 10min at 150 ℃ to complete powder coating modification;
(2) uniformly mixing the coated and modified zirconia powder and a binder in an internal mixer according to a proportion, preparing a feed, crushing, and then extruding and granulating by using a single-screw extruder to prepare the high-density zirconia powder injection molding special material.
6. The method for preparing the high-density zirconia powder injection molding special material according to claim 5, wherein the temperature of the internal mixer in the step (2) is set to 180 ℃, and the rotating speed is 30 r/min; banburying twice for 10 minutes each time.
7. The method for preparing the high-density zirconia powder injection molding special material according to claim 5, wherein the temperature of the single-screw extruder in the step (2) is set as follows: 150 ℃, 160 ℃, 170 ℃, 175 ℃, 180 ℃, 180 ℃, and the rotation speed of 150 ℃ and 200 rpm.
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