CN105503181A - Preparation method for yttria-stabilized zirconia powder - Google Patents
Preparation method for yttria-stabilized zirconia powder Download PDFInfo
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Abstract
The invention relates to a preparation method for yttria-stabilized zirconia powder. The method comprises the steps that zirconium oxychloride and yttrium nitrate are added into a polyvinyl alcohol solution, the mixture is stirred to be uniform, then a glutaraldehyde solution is added, and the mixture is stirred for 8-15 min at the temperature of 40-50 DEG C to obtain gel, wherein the molar ratio of zirconium oxychloride to yttrium nitrate is 97 to 3; the gel is taken out for standing before being cut into blocks, placed in ammonium hydroxide to be soaked for 15-20 hours and then dried and calcined to obtain the yttria-stabilized zirconia powder. Through the preparation method for the yttria-stabilized zirconia powder, formed zirconia crystal nuclei grow in a cross-linking network provided by polyvinyl alcohol gel liquid; due to limitation of the three-dimensional network, zirconia particles can be prevented from colliding with one another and gathering, agglomeration is reduced, and the yttria-stabilized zirconia powder with a small particle size and good uniformity can be obtained conveniently.
Description
Technical field
The present invention relates to zirconia ceramics technical field, particularly relate to a kind of preparation method of Zirconium powder of stabilized with yttrium oxide.
Background technology
As novel high-performance ceramics, zirconia ceramics has the attribute such as heat-proof quality and resistance to elevated temperatures of high strength, high-fracture toughness, high rigidity and excellence, is widely used in structural ceramics and function ceramics field.In addition, zirconium white does not have magnetic, non-conductive, non-corrosive, wear-resisting, and it also applies very wide in biomedical apparatus field and stage property, field of tool.Recently, PSZ (TZP) can pass through powder metallurgy process, and preparation keeps away the wristwatch case of magnetic, the table part of corrosion resistant and Other Instruments part.Except above-mentioned application, TZP is also widely used in the fields such as decoration, life, medical science, piezoelectric ceramics, sensor pottery.
First Stupalox is succeeded in developing by Kyocera and is put on market, and being just subject to the favor of people once appearance and pursuing, is high-tech product in recent years.Plump glossy as the unique jade of zirconia ceramic knife, fashionable, is known as " noble's cutter ".Its keen edge is incomparable, and wear resistance is higher than steel knife tens times, can be rated as " never wornout ".Zirconia ceramics has that chemical stability is high, acid-alkali-corrosive-resisting, easy cleaning non-corrosive, cut the characteristics such as thing free from extraneous odour, is typical " Green Product ".
But also there is the technical need improved further in the material oxidation zirconium raw powder's production technology of current zirconia ceramic knife.
Summary of the invention
Based on this, be necessary for the problems referred to above, the preparation method of the Zirconium powder of a stabilized with yttrium oxide is provided, obtain the less and equally distributed Zirconium powder of particle diameter.
A preparation method for the Zirconium powder of stabilized with yttrium oxide, comprises the steps:
Add in polyvinyl alcohol solution by zirconium oxychloride, Yttrium trinitrate, after stirring, add glutaraldehyde solution, be stir 8 ~ 15min under the condition of 40 ~ 50 DEG C in temperature, obtain gel, wherein, the mol ratio of zirconium oxychloride and Yttrium trinitrate is 97:3;
Described gel is taken out, stripping and slicing after leaving standstill, and after being placed in ammoniacal liquor immersion 15 ~ 20h, drying, calcine, obtain the Zirconium powder of stabilized with yttrium oxide.
Wherein in an embodiment, the concentration of described polyvinyl alcohol solution is 2% ~ 5%.
Wherein in an embodiment, the concentration of described glutaraldehyde solution is 20% ~ 30%.
Wherein in an embodiment, the volume ratio of described polyvinyl alcohol solution and described glutaraldehyde solution is 4 ~ 6:1.
Wherein in an embodiment, the mass ratio of described zirconium oxychloride and polyvinyl alcohol solution is 1:2 ~ 3.
Wherein in an embodiment, the temperature of described oven dry is 75 ~ 85 DEG C.
Wherein in an embodiment, the temperature of described calcining is 600 DEG C.
Wherein in an embodiment, described gel is cut into 1 ~ 3cm
3lumphy structure be placed in ammoniacal liquor and soak.
The preparation method of the Zirconium powder of above-mentioned stabilized with yttrium oxide, forms crosslinked between macromolecular chain by the hydroxyl reaction in glutaraldehyde and polyvinyl alcohol macromolecular chain and forms countless three-dimensional net structure, after zirconium oxychloride joins polyvinyl alcohol water solution, and Zr
4+formation with gel is just fixed in three-dimensional net structure; soak and drying and processing through ammoniacal liquor; the zirconium white nucleus formed grows in the cross-linked network that polyvinyl alcohol gel liquid provides; owing to being subject to the restriction of three-dimensional network; can prevent zirconia particles from colliding with each other, assemble and reduce the generation of reunion, be conducive to obtaining that particle diameter is less, the Zirconium powder of the good stabilized with yttrium oxide of homogeneity.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the preparation method of sintex in one embodiment of the invention;
Fig. 2 is the schematic flow sheet of the preparation method of the Zirconium powder of stabilized with yttrium oxide in one embodiment of the invention;
Fig. 3 is the schematic flow sheet of the preparation method of zirconia ceramics pelletizing in one embodiment of the invention.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public specific embodiment.
Unless otherwise defined, all technology used herein and scientific terminology are identical with belonging to the implication that those skilled in the art of the present invention understand usually.The object of term used in the description of the invention herein just in order to describe specific embodiment, is not intended to be restriction the present invention.Term as used herein "and/or" comprises arbitrary and all combinations of one or more relevant Listed Items.
Refer to Fig. 1, it is the schematic flow sheet of the preparation method of sintex in one embodiment of the invention.
Such as, the preparation method of sintex, comprises the steps:
The preparation of the Zirconium powder of S100, stabilized with yttrium oxide.
Concrete, refer to Fig. 2, the preparation method of the Zirconium powder of stabilized with yttrium oxide, comprises the steps:
S110, zirconium oxychloride, Yttrium trinitrate are added in polyvinyl alcohol solution, after stirring, add glutaraldehyde solution, be stir 8 ~ 15min under the condition of 40 ~ 50 DEG C in temperature, obtain Zr
4+organic network gel.
Be appreciated that, after polyvinyl alcohol is water-soluble, the macromolecular chain being in winding state can extend gradually, now solution fill by the swelling macromole ball of string, the crosslinked action of macromolecular chain accounts for leading, simultaneously, it is crosslinked that hydroxyl reaction on glutaraldehyde and presoma polyvinyl alcohol macromolecular chain is formed between macromolecular chain, and cross linked chain stretches the countless three-dimensional net structure of formation intricately, after zirconium oxychloride is joined polyvinyl alcohol water solution, Zr
4+formation with gel is just fixed in three-dimensional net structure, forms Zr
4+organic network gel.
Such as, the mol ratio of zirconium white and Yttrium trinitrate is 97:3, and can prepare 3mol% yttrium stable zirconium oxide powder (3YSZ), its practical value is higher.
And for example, the concentration of described polyvinyl alcohol solution is 2% ~ 5%.Preferably, the concentration of described polyvinyl alcohol solution is 2% ~ 3%, along with the increase of the concentration of polyvinyl alcohol, gel-strength increases gradually, and without cracking, bleed phenomenon, and the increase of gel-strength, then can affect the velocity of diffusion of ammoniacal liquor when follow-up ammoniacal liquor soaks, to soaking technology and last calcining row carbon process unfavorable, cause calcining temperature to raise.
And for example, the concentration of described glutaraldehyde solution is 20% ~ 30%.And for example, the volume ratio of described polyvinyl alcohol solution and described glutaraldehyde solution is 4 ~ 6:1.Preferably, the concentration of described glutaraldehyde solution is 25%, and the volume ratio of described polyvinyl alcohol solution and described glutaraldehyde solution is 5:1, when the concentration of glutaraldehyde is lower, glutaraldehyde and the more difficult generation crosslinking reaction of polyvinyl alcohol, the speed making gel be difficult to be formed or formed is slower, because the hydroxyl reaction in glutaraldehyde and polyvinyl alcohol molecule chain forms cross linked chain, improve polyvinyl alcohol macromolecular chain, but destroy the interaction of a large amount of hydrogen bond between polyvinyl alcohol macromolecular chain simultaneously, gel-strength is reduced.When glutaraldehyde concentration increases, can gel time be shortened, but when the concentration of glutaraldehyde is more than 30%, then gel can be made instantaneously gelling to occur, affect stability and the subsequent operations process of system.
And for example, the mass ratio of described zirconium oxychloride and polyvinyl alcohol solution is 1:2 ~ 3.Further, the mass ratio of described zirconium oxychloride and polyvinyl alcohol solution is 1:2.5 ~ 2.8, is appreciated that when after gel formation, Zr
4+just be fixed in the three-dimensional network body that is made up of polyvinyl alcohol and glutaraldehyde cross-linking, as starting inorganic Zr
4+when ionic concn is lower, there are enough network microcells for its attachment, along with Zr
4+the increase of ionic concn, in the free water just having unnecessary ion to be free in gelling system, the ionic concn due to three-dimensional network microcell is greater than extraneous ionic concn, namely there is concentration difference, diffusion phenomena occurs thereupon, cause gel piece strength degradation.Thus causing the cracking of gel, water molecules just can be separated out along with crack, occurs bleeding.When the amount that zirconium oxychloride adds is larger, the stability of gel can be destroyed, make Gel Tear, bleed, cause Zr
4+loss, and when the amount that zirconium oxychloride adds is less, then the intensity of gel can be made to reduce, cause Gel Tear, bleed.
And for example, be stir under the condition of 45 DEG C in temperature, when temperature is lower, the gelation time of needs is longer, and when temperature is higher, then can affect the stability of gel.
And for example, stirring velocity is 1200 ~ 1500rpm, and stirring velocity is less, stirs uneven, cause gel uneven, and stirring velocity is excessive, then make the speed of gel formation slower.
And for example, after adding glutaraldehyde, the pH controlling reaction system is 2.0 ~ 9.0, and along with the increase of system pH, gelation rate is too fast, as pH < 2.0, gelation rate and dewatering speed too fast, dehydrating amount is excessive, as pH > 9.0, then have precipitation to generate, affect the formation of gel.Preferably, after adding glutaraldehyde, the pH controlling reaction system is 2.0 ~ 4.0, and the time of system gelation is less with the change fluctuation of pH, and gelation process easily controls, and the gel-strength formed is better.
A good example is, measures the polyvinyl alcohol solution 1L that concentration is 2% ~ 3%, adds 700gZrOCl successively
28H
2o and 25gY (NO
3)
26H
2o, stirring velocity is stir under the condition of 1200 ~ 1500rpm/min, and after stirring, instillation concentration is the glutaraldehyde 200mL of 25%, and continuing to stir, is thermostatically heating 10min in the water-bath of 45 DEG C in temperature, leaves standstill, obtains Zr
4+organic network gel.
S120, described gel to be taken out, stripping and slicing after leaving standstill, and is placed in after ammoniacal liquor soaks 15 ~ 20h, dry, calcining, obtain the Zirconium powder of stabilized with yttrium oxide.
After immersing ammonia soln, zirconium oxychloride and Yttrium trinitrate are under alkaline environment, and precipitin reaction occurs, and reaction formula is as follows:
ZrOCl
2+2NH
4OH+H
2O→Zr(OH)
4↓+2NH
4C1
Y(NO
3)
3+3NH
4OH→Y(OH)
3↓+3NH
4NO
3
Further, generating zirconium hydroxide and yttrium hydroxide to fully make the zirconium oxychloride in gel and Yttrium trinitrate and ammoniacal liquor react, such as, described gel being taken out, after leaving standstill, be cut into 1 ~ 3cm
3lumphy structure, like this, the contact area of gel and ammoniacal liquor can be increased, make zirconium oxychloride and Yttrium trinitrate be converted into zirconium hydroxide and yttrium hydroxide.
Further, be precipitated out in order to ensure zirconium hydroxide and yttrium hydroxide simultaneously, such as, stirring operation is carried out to ammoniacal liquor during immersion simultaneously, and for example, described stirring operation adopts magnetic stirring apparatus to carry out, and its mixing effect is more even, thus can guarantee that zirconium hydroxide and yttrium hydroxide are precipitated out simultaneously further.
Further, in order to remove the impurity of gel surface, such as, after being taken out from ammoniacal liquor by gel, carry out water washing operations, not only effectively can eliminate the impurity of gel surface, eliminate agglomeration traits as much as possible.And for example, described washing adopts deionized water to clean, and like this, can avoid introducing all the other ions.
Such as, the temperature of oven dry is 75 ~ 85 DEG C, and preferably, the temperature of oven dry is 80 DEG C, to slough the free-water of gel surface.
Further, in order to obtain the good Zirconium powder of quality, such as, gel powder after oven dry is placed in High Temperature Furnaces Heating Apparatus calcine, when temperature is 25 DEG C ~ 300 DEG C, with the temperature rise rate of 3 DEG C/min, namely per minute heats up 3 DEG C, to remove free water in gel and ammonium salt, and 1h is kept 300 DEG C time, to remove the polyvinyl alcohol in gel, and then be heated to 600 DEG C of isothermal calcining 2h with the temperature rise rate of 5 DEG C/min, the Zirconium powder obtained after completing calcining is come out of the stove to room temperature along with the cooling down of High Temperature Furnaces Heating Apparatus, like this, the Zirconium powder size of microcrystal that obtains can be made less, monodispersity is better, be more evenly distributed, promote the quality of Zirconium powder.Such as, the gel powder after drying is placed in before High Temperature Furnaces Heating Apparatus calcines, also comprises step: to spend the night placement in dry environment, such as, to spend the night placement at freeze-day with constant temperature environment; Wherein, spend the night described in be placed as and at least leave standstill 6 hours; And for example, described constant temperature is 20 to 30 degrees Celsius.Such process, is conducive to the free water molecule removed further in gel, promotes the uniform particle diameter of calcinate and reduces particle diameter length.
Due to Zr
4+be fixed in three-dimensional network microcell, during ammonia treatment, OH
-just to penetrate into gradually in gel network microcell and and Zr
4+in conjunction with formation Zr (OH)
4nH
2in O organic network body, be heated in calcining temperature process, organic network stereoeffect can not move, the Zr (OH) in each small grid
4nH
2the intermolecular distance of O is relatively far away, does not also have enough time to reunite, and just decomposes in position, and release water vapour, like this, the Zirconium powder particle diameter of generation can be made less, and homogeneity is better.
The preparation method of the Zirconium powder of above-mentioned stabilized with yttrium oxide, forms crosslinked between macromolecular chain by the hydroxyl reaction in glutaraldehyde and polyvinyl alcohol macromolecular chain and forms countless three-dimensional net structure, after zirconium oxychloride joins polyvinyl alcohol water solution, and Zr
4+formation with gel is just fixed in three-dimensional net structure; soak and drying and processing through ammoniacal liquor; the zirconium white nucleus formed grows in the cross-linked network that polyvinyl alcohol gel liquid provides; owing to being subject to the restriction of three-dimensional network; can prevent zirconia particles from colliding with each other, assemble and reduce the generation of reunion, be conducive to obtaining that particle diameter is less, the Zirconium powder of the good stabilized with yttrium oxide of homogeneity.
In addition, the preparation method of the Zirconium powder of above-mentioned stabilized with yttrium oxide, by adding Yttrium trinitrate, Y
3+ion can enter in zirconic lattice, replaces Zr
4+ion, form substitutional solid solution, make Zirconium powder with Tetragonal stable existence, make it have the good characteristic such as heat-resisting, corrosion-resistant, toughness reinforcing, and yttrium oxide can stablize tetragonal phase zirconium oxide in wider scope, the stability of Zirconium powder effectively can be improved.
The preparation of S200, zirconia ceramics pelletizing.
Concrete, refer to Fig. 3, the preparation method of zirconia ceramics pelletizing, comprises the steps:
S210, by the Zirconium powder of described stabilized with yttrium oxide, dispersion agent, antiseptic-germicide and deionized water mixing after ball milling make slurry.
Concrete, in order to improve zirconic density, reduce sintering temperature, such as, in Zirconium powder, add aluminum oxide, and for example, the mass ratio of described Zirconium powder and described aluminum oxide is 100:0.1 ~ 0.6, by adding aluminum oxide, can the densification of accelerating oxidation zirconium powder body, reduce sintering temperature.Preferably, aluminum oxide is nanoparticle, and its particle diameter is 10 ~ 20nm.
Further, the mass ratio of described Zirconium powder and described antiseptic-germicide is 100:3 ~ 5.Further, described antiseptic-germicide is the composition of silver suboxide, Palladous chloride, copper sulfate and zinc chloride.Further, the mass ratio of silver suboxide, Palladous chloride, copper sulfate and zinc chloride is 1:0.05 ~ 0.1:0.5 ~ 1:0.2 ~ 0.5.By regulating the ratio of each component in antiseptic-germicide, making the antimicrobial spectrum of antiseptic-germicide more wide, improving the anti-microbial property of antiseptic-germicide.In one embodiment of the invention, the preparation method of antiseptic-germicide is: in mass ratio silver suboxide, Palladous chloride, copper sulfate and zinc chloride and tackiness agent and deionized water are added ball milling 1 ~ 2h in ball mill successively, sieve, make antiseptic-germicide slurry; By the slip casting of antiseptic-germicide slurry, at the temperature of 1100 ~ 1300 DEG C, sinter 50 ~ 80min, to remove tackiness agent and water; Fragmentation, and crossing after 200 mesh sieves, is placed in ball mill and carries out second time ball milling and obtain antiseptic-germicide.
Further, in order to improve the anti-microbial property of antiseptic-germicide, such as, also comprise nano titanium oxide in antiseptic-germicide, the mass ratio of described nano titanium oxide and silver suboxide is 1:1 ~ 1.2, and nano titanium oxide can make bacterial degradation and reach antibacterial effect under photocatalysis, and silver suboxide can at nano titanium oxide surface deposition negatively charged ion, isolate photo-generated carrier, improve the photocatalytic activity of nano titanium oxide, improve the anti-microbial property of antiseptic-germicide further.Such as, when the mass ratio of described nano titanium oxide and silver suboxide is 1:1.15, silver suboxide deposition effect is better.
Further, in order to improve the uniformity coefficient of zirconia ceramics pelletizing, reduce its particle diameter, such as, the particle diameter of Zirconium powder is 10 ~ 20nm, and the particle diameter of antiseptic-germicide is 10 ~ 50nm, by the particle diameter of controlled oxidization zirconium powder body and antiseptic-germicide, less with the slurry particle diameter obtained after making ball milling, be conducive to the uniformity coefficient improving zirconia ceramics pelletizing, reduce its particle diameter.
Further, be the ratio mixing of 1:1 ~ 1.2 in solid-to-liquid ratio by described Zirconium powder, aluminum oxide, dispersion agent, antiseptic-germicide and deionized water, namely, the total mass of Zirconium powder, aluminum oxide, dispersion agent, antiseptic-germicide and the mass ratio of deionized water are 1:1 ~ 1.2, be placed in ball mill to carry out ball milling and make slurry, the slurry after ball milling can be made to have suitable solid content, be conducive to follow-up granulation process, make the pelletizing regular shape after granulation, suppression performance is good.
Further, ball milling adopts ball mill to carry out stirring wet ball grinding, further, the rotating speed of ball mill is 500 ~ 1000rpm, and the time of ball milling is 1 ~ 2h, like this, the particle diameter of the slurry after ball milling can be made more evenly regular, contribute to follow-up granulation and sintering process.
Further, in order to reduce follow-up sintering temperature, improve the density of Stupalox, such as, the median size of the described slurry after ball milling is 0.5 ~ 0.8 micron, preferably, the median size of the described slurry after ball milling is 0.5 ~ 0.6 micron, like this, the slurry after ball milling can be made to have higher surface energy, to make the pelletizing after granulation have higher sintering activity, and then reduce follow-up sintering temperature, also can improve the density of obtained ceramic simultaneously.
In the present embodiment, dispersion agent is at least one in ammonium polyacrylate, sodium polyacrylate, ammonium citrate and glycerol.By adding dispersion agent, interparticle reunion can be reduced, to realize the effect of ball milling better.
S220, add binding agent by described slurry, after stirring, granulation, obtains zirconia ceramics pelletizing;
Such as, described binding agent is at least two kinds in polyvinyl alcohol, polyoxyethylene glycol and Xylo-Mucine.And for example, the mass ratio of described binding agent and described slurry is 1:80 ~ 150.And for example, the mass ratio of described binding agent and described slurry is 1:100 ~ 120.Like this, the nucleation rate of slurry can be improved, reduce the coarsening rate of pelletizing, make pelletizing particle diameter little and even.
Further, in order to make binding agent fully mix with slurry, such as, after adding binding agent, stir 3 ~ 8h, and for example, stir 4 ~ 6h after adding binding agent, binding agent both can have been made fully to mix with slurry, effectively can also provide production efficiency.
In the present embodiment, sponging granulator mist projection granulating is adopted.Such as, mist projection granulating adopts atomizer mode.Concrete, the slurry be stirred pumps into mist projection granulating in sponging granulator by charging pump.When adopting sponging granulator mist projection granulating, the intake air temperature of sponging granulator is 220 DEG C ~ 250 DEG C, and air outlet temperature is 110 DEG C ~ 120 DEG C, and the rotating speed of spraying gun is 7000rpm ~ 9000rpm, and charging pump frequency is 25Hz ~ 50Hz.By controlling the condition of sponging granulator, the pelletizing particle diameter that obtains can be made less and homogeneity is better.
Further, in order to improve the suppression performance of pelletizing, such as, to make the Stupalox obtained have good compactness, after slurry is carried out granulation, also comprise the step of being carried out by pelletizing sieving.And for example, by being sieved under 80 object screen clothes by pelletizing, the minus mesh of collection is pelletizing, like this, can improve the uniformity coefficient of pelletizing, improves the suppression performance of pelletizing, has good compactness to make the Stupalox obtained.
The preparation method of above-mentioned zirconia ceramics pelletizing, owing to adding antiseptic-germicide, the pelletizing obtained can be made to have antibacterial efficacy, and by adding dispersion agent and binding agent respectively in preparation process, can make the zirconia ceramics pelletizing regular shape obtained, output capacity is higher.
The preparation of S300, finished product.
Concrete, it comprises the steps:
S310, described zirconia ceramics pelletizing is carried out premolding compacting, then carry out isostatic pressed process, obtain green compact.
Such as, described zirconia ceramics pelletizing is placed in mould and carries out dry-pressing compacting, concrete, according to shape and the size mfg. moulding die of sintex, zirconia ceramics pelletizing is placed in mould dry-pressing and is pressed into the base substrate with the shape of tool, then base substrate is placed in static pressure machine and carries out isostatic pressed process, so that base substrate compacting is fine and close, obtain green compact.
Further, the pressure of premolding compacting is 200 ~ 300kg/cm
2, the time of premolding compacting is 3 ~ 5min, that is, be 200 ~ 300kg/cm at pressure
2when keep 3 ~ 5min, release, after depanning, through polishing shaping, obtain molding blank.
Further, in order to make the sintex obtained have higher density, to improve its toughness, such as, the pressure waiting pressing process quietly is 1400 ~ 1600kg/cm
2green compact can be made can to obtain more effective extruding, the green compact obtained are made to have higher compactness, thus make sintex finished product have better intensity and toughness, the sintering temperature that the green compact that compactness is high simultaneously need is lower, decrease the energy consumption of sintering, reduce production cost and be conducive to environmental protection.It should be noted that, when force value is more than 1600kg/cm
2time, along with the increase density of pressure increases not obvious, and higher to the requirement of equipment.
S320, described green compact to be sintered, obtain blank.
Such as, the temperature of described sintering is 1300 ~ 1600 DEG C.And for example, the temperature of described sintering is 1450 ~ 1500 DEG C.And for example, the time of described sintering is 2 ~ 4h.
Further, in order to obtain the higher blank of density, such as, green compact are placed in High Temperature Furnaces Heating Apparatus and are heated to 600 DEG C with the temperature rise rate of 3 DEG C/min, and 600 DEG C time, keep 1h to remove no-bonder and dispersion agent, then be heated to 1450 ~ 1500 DEG C with the temperature rise rate of 10 DEG C/min, isothermal sintering 2 ~ 4h, cools to room temperature with the furnace after sintering.Be appreciated that, when sintering temperature is lower than 600 DEG C, the mainly eliminating of moisture and the burn off process of binding agent in base substrate, along with the raising of sintering temperature, the shrinking percentage of base substrate increases gradually, but the speed increased is slower, when sintering temperature reaches more than 1200 DEG C, base substrate shrinking percentage increases suddenly, and base substrate inner air vent is got rid of rapidly, reaches densification.Preferably, in order to improve the density of blank further, such as, green compact are placed in High Temperature Furnaces Heating Apparatus and are heated to 600 DEG C with the temperature rise rate of 3 DEG C/min, and 600 DEG C time, keep 1h to remove no-bonder and dispersion agent, then 1200 DEG C are heated to the temperature rise rate of 10 DEG C/min, be warming up to the temperature rise rate of 3 ~ 5 DEG C/min, isothermal sintering 2 ~ 4h, cools to room temperature with the furnace after sintering again, to make the pore in base substrate fully get rid of, make the blank density that obtains higher.
S330, described blank carried out polish, polishing, to put the first edge on a knife or a pair of scissors, obtain sintex.
Concrete, the blank after sintering is undertaken roughly grinding, refining by grinding wheel.During polishing, blank is put into polishing machine, adds polishing fluid simultaneously and carry out mirror polish, to improve the appearance effect of sintex.
The preparation method of above-mentioned antibacterial ceramic cutter, can make the sintex consistent internal structure obtained, density is higher, and bending strength is higher, and toughness is better, and processing rear knife edge is sharp, and owing to adding antiseptic-germicide, can make its good anti-microbial property.
Each technical characteristic of the above embodiment can combine arbitrarily, for making description succinct, the all possible combination of each technical characteristic in above-described embodiment is not all described, but, as long as the combination of these technical characteristics does not exist contradiction, be all considered to be the scope that this specification sheets is recorded.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be construed as limiting the scope of the patent.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (8)
1. a preparation method for the Zirconium powder of stabilized with yttrium oxide, is characterized in that, comprises the steps:
Add in polyvinyl alcohol solution by zirconium oxychloride, Yttrium trinitrate, after stirring, add glutaraldehyde solution, be stir 8 ~ 15min under the condition of 40 ~ 50 DEG C in temperature, obtain gel, wherein, the mol ratio of zirconium oxychloride and Yttrium trinitrate is 97:3;
Described gel is taken out, stripping and slicing after leaving standstill, and after being placed in ammoniacal liquor immersion 15 ~ 20h, drying, calcine, obtain the Zirconium powder of stabilized with yttrium oxide.
2. the preparation method of the Zirconium powder of stabilized with yttrium oxide according to claim 1, is characterized in that, the concentration of described polyvinyl alcohol solution is 2% ~ 5%.
3. the preparation method of the Zirconium powder of stabilized with yttrium oxide according to claim 2, is characterized in that, the concentration of described glutaraldehyde solution is 20% ~ 30%.
4. the preparation method of the Zirconium powder of stabilized with yttrium oxide according to claim 3, is characterized in that, the volume ratio of described polyvinyl alcohol solution and described glutaraldehyde solution is 4 ~ 6:1.
5. the preparation method of the Zirconium powder of stabilized with yttrium oxide according to claim 1, is characterized in that, the mass ratio of described zirconium oxychloride and polyvinyl alcohol solution is 1:2 ~ 3.
6. the preparation method of the Zirconium powder of stabilized with yttrium oxide according to claim 1, is characterized in that, the temperature of described oven dry is 75 ~ 85 DEG C.
7. the preparation method of the Zirconium powder of stabilized with yttrium oxide according to claim 1, is characterized in that, the temperature of described calcining is 600 DEG C.
8. the preparation method of the Zirconium powder of stabilized with yttrium oxide according to claim 1, is characterized in that, described gel is cut into 1 ~ 3cm
3lumphy structure be placed in ammoniacal liquor and soak.
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| CN107619066A (en) * | 2017-10-25 | 2018-01-23 | 福建省智胜矿业有限公司 | A kind of zirconia powder preparation process of magnesium stable composition |
| CN110002496A (en) * | 2019-02-25 | 2019-07-12 | 王召惠 | A kind of anti-preparation method for peeling off zirconia coating Zirconium oxide powder |
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| CN110002496A (en) * | 2019-02-25 | 2019-07-12 | 王召惠 | A kind of anti-preparation method for peeling off zirconia coating Zirconium oxide powder |
| CN110078499A (en) * | 2019-05-16 | 2019-08-02 | 金业新材料科技(昆山)有限公司 | A kind of water system PMMA dry-pressing/isostatic pressing prilling powder and preparation method thereof |
| CN110590407A (en) * | 2019-09-27 | 2019-12-20 | 合肥汉甲陶瓷科技有限公司 | Firing method for uniformly distributing cracks on surface of crack glaze ceramic |
| CN110590407B (en) * | 2019-09-27 | 2020-11-06 | 福建省德化县雅丽达陶瓷有限公司 | Firing method for uniformly distributing cracks on surface of crack glaze ceramic |
| CN110586058A (en) * | 2019-10-10 | 2019-12-20 | 河南科技大学 | Preparation method of nano titanium dioxide/zirconium oxide composite photocatalyst |
| CN111106336A (en) * | 2019-12-23 | 2020-05-05 | 江苏理工学院 | Preparation method of ZnO/C nano composite material, electrode plate and soft package NiZn battery |
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