CN103319173A - Method for preparing zirconia ceramic microbead in rolling molding mode - Google Patents
Method for preparing zirconia ceramic microbead in rolling molding mode Download PDFInfo
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- CN103319173A CN103319173A CN2013102668535A CN201310266853A CN103319173A CN 103319173 A CN103319173 A CN 103319173A CN 2013102668535 A CN2013102668535 A CN 2013102668535A CN 201310266853 A CN201310266853 A CN 201310266853A CN 103319173 A CN103319173 A CN 103319173A
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Abstract
The invention relates to a method for preparing zirconia ceramic microbeads in a rolling molding mode. The method comprises the following steps of: (1) dispersing yttria-stabilized zirconia powder/cerium-stabilized zirconia powder; (2) adding yttria-stabilized zirconia powder/cerium-stabilized zirconia powder and mixed glue into a sugarcoating machine in a mode that the materials are added and the glue is sprayed at the same time, and generating zirconia ceramic microbread green bodies in the rolling molding mode; (3) preserving the temperature of the zirconia ceramic microbread green bodies at 1,400-1,550 DEG C for 3-6 hours, and sintering the green bodies into zirconia ceramic microbread rough blanks; (4) polishing the zirconia ceramic microbread rough blanks so as to obtain the zirconia ceramic microbeads. Through dispersion, the yttria-stabilized zirconia powder/cerium-stabilized zirconia powder is uniformly dispersed into independent grains, the zirconia ceramic microbread green bodies are generated by using the rolling molding method, the zirconia ceramic microbread green bodies are sintered at the temperature of 1,400-1,550 DEG C, and finally the polishing treatment is carried out; the prepared zirconia ceramic microbeads are solid and wear-resisting.
Description
Technical field
The present invention relates to a kind of manufacture method of stupalith, relate in particular to the method that a kind of moulding of rolling prepares the zirconia ceramics microballon.
Background technology
Along with the superfine powder demand is more and more vigorous, also larger for the demand of the following specification grinding medium of 3mm.Zirconia ceramics is because it wear-resisting, corrosion-resistant, resistance to elevated temperatures that possesses is widely used in grinding industry.Adopt traditional preparation technology, can't satisfy the requirement of its wear resisting property or dimensions such as dry-pressing technique, therefore in the urgent need to prepare wear-resisting small dimension zirconia ceramics grinding medium with a kind of novel process.
Summary of the invention
The technical problem to be solved in the present invention provides the method that a kind of moulding of rolling prepares the zirconia ceramics microballon, and the method that this rolling moulding prepares the zirconia ceramics microballon can produce more wear-resisting zirconia ceramics microballon.The technical scheme that adopts is as follows:
A kind of moulding of rolling prepares the method for zirconia ceramics microballon, it is characterized in that comprising the steps:
(1), yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder is disperseed;
(2), in the mode while the glue spraying of feeding in raw material, yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder and epoxy glue are joined in the coater, generate zirconia ceramics microballon green compact by the rolling moulding;
(3), zirconia ceramics microballon green compact are incubated 3～6 hours under 1400 ℃～1550 ℃ temperature, sinter zirconia ceramics microballon blank into;
(4), zirconia ceramics microballon blank is polished, obtain finished product zirconia ceramics microballon.
By disperseing, making yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder Uniform Dispersion is individual particles, method by the rolling moulding generates zirconia ceramics microballon green compact again, sintering under 1400 ℃～1550 ℃ temperature again, carry out at last polished finish, the zirconia ceramics microballon of making is more solid, more wear-resisting.
As preferred version of the present invention, described yttrium stable zirconium oxide powder is by Y
20
3And Zr(Hf) O
2The compound zirconium powder material that forms, each compositions in weight percentage is: Y
20
34.9～5.5%, Zr(Hf) O
294.5～95.1%; Described cerium stabilizing zirconium oxide powder is by CeO
2And Zr(Hf) O
2The compound zirconium powder material that forms, each compositions in weight percentage is: CeO
26～20%, Zr(Hf) O
280～94%.
As preferred version of the present invention, described epoxy glue is formulated by PVA, paraffin, CMC, oleic acid and deionized water, and the summation of PVA, paraffin, CMC, oleic acid and the weight ratio of deionized water are (0.01～0.02): 1.The epoxy glue that adopts PVA, paraffin, CMC, oleic acid and deionized water to be mixed with, viscosity is high, is fit to the bonding of yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder, and is quite firm after the bonding.
As the further preferred version of the present invention, described yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder is by the preparation of ball milling granulation process.The ball milling granulation process mainly is to produce the powder material by ball mill, and the yttrium stable zirconium oxide powder of making thus/cerium stabilizing zirconium oxide powder has even-grained characteristics.
As the further preferred version of the present invention, described yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder disperses by micronizer mill, the pressure of micronizer mill is equal to or greater than 1.0Mpa, and reinforced air pressure is 0.2～1.0Mpa, and feed rate is 0.05～0.5 kg/minute.Adopt micronizer mill that yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder is disperseed, almost all particles can be spread out fully, improve final product quality and yield rate.
As the further preferred version of the present invention, described step (2) specifically comprises generation zirconia ceramics microballon kind substep and generates zirconia ceramics microballon green compact step;
Generating zirconia ceramics microballon kind substep comprises:
(2-1-1), start coater, the rotating speed of coater is controlled at 15～45 rev/mins;
(2-1-2), yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder is disperseed simultaneously, slowly to add epoxy glue in the coater by spray gun in the adding coater;
(2-1-3), the moulding of in coater, rolling, be the zirconia ceramics microballon seed that 0.02mm is above and have higher hardness until generate diameter, then take out;
Generating zirconia ceramics microballon green compact step comprises:
(2-2-1), start coater, the rotating speed of coater is controlled at 15～45 rev/mins;
(2-2-2), with disposable the joining in the coater of zirconia ceramics microballon seed that step (2-1-3) generates, simultaneously, slowly add epoxy glue in the coater by spray gun;
(2-2-3), in the rolling moulding process, adopt diverting device that the zirconia ceramics microballon seed that is stained with epoxy glue is disperseed;
(2-2-4), after zirconia ceramics microballon seed disperses, in coater, disperse to add yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder, continue the rolling moulding, until zirconia ceramics microballon seed is with bonding solid with yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder;
(2-2-5), by spray gun epoxy glue is slowly added in the coater, then continue performing step (2-2-3), (2-2-4), until the diameter of the zirconia ceramics microballon green compact that generate reaches till the requirement.
As the present invention's preferred version further, described diverting device comprises support, draws together tilting mechanism, connecting rod, swing seat, soft of many plastics, elevating bracket and arrangement for adjusting height; Elevating bracket is rack-mount and can be on support slide along the vertical direction, and arrangement for adjusting height is rack-mount, and the clutch end of arrangement for adjusting height is connected with elevating bracket, and tilting mechanism is installed on the elevating bracket; One end of connecting rod is connected with the clutch end of tilting mechanism, and the other end of connecting rod is connected with swing seat; Soft of plastics are installed on the swing seat.In the production process of zirconia ceramics microballon, swing as tilting mechanism drive link drive swing seat such as the pendulum, soft of plastics on the swing seat are back and forth stirred powder and coccoid green compact back and forth, powder or coccoid green compact are spread out, to connect the ball rate is reduced in 1% from 30%, made simultaneously the balling-up Speed improving about 40%, therefore, this swing diverting device can reduce in the production process of zirconia ceramics microballon and connects the ball rate, improves balling-up speed, improves the balling-up quality.Arrangement for adjusting height comprises mounting block and screw rod, and mounting block is installed on the described support, offers through hole along the vertical direction on the mounting block, offers screw along the vertical direction on the elevating bracket, and screw rod is in through hole and the screw.Tilting mechanism is oscillating cylinder, and described oscillating cylinder comprises cylinder body, gear, two pistons, two tooth bars and swing axle; Gear is installed in the cylinder body and is in the middle part of cylinder body; Two pistons are installed in the cylinder body and are in the both sides of gear; Article two, an end of tooth bar is connected with corresponding piston respectively, and two tooth bars all are meshed with gear; One end of swing axle is connected with gear is coaxial.Swing axle is as the clutch end of oscillating cylinder.
As the present invention's preferred version further again, the dual-side that described plastics are soft is spline-simulating.
As the further preferred version of the present invention, the inboard wall of cylinder block of described coater is coated with the uniform polyurethane coating of a layer thickness.
As the present invention's preferred version further, in the described step (4), adopt the aluminum oxide radioceramic to polish as polishing medium.
Description of drawings
Fig. 1 is the schematic flow sheet of the preferred embodiment for the present invention;
Fig. 2 is the structural representation of diverting device;
Fig. 3 is the structural representation of oscillating cylinder.
Embodiment
Be described further below in conjunction with accompanying drawing and preferred implementation of the present invention.
As shown in Figure 1, this rolling moulding prepares the method for zirconia ceramics microballon, it is characterized in that comprising the steps:
(1), the yttrium stable zirconium oxide powder is disperseed, the pressure of micronizer mill is that the general pressure of 1.0Mpa(is greater than 1.0Mpa), reinforced air pressure is 0.5 Mpa (in the scope of 0.2～1.0Mpa can), feed rate is 0.2 kg/minute (in the scope of 0.05～0.5 kg/minute can), wherein, the yttrium stable zirconium oxide powder is by 4.9% Y
20
3With 95.1% Zr(Hf) O
2The compound zirconium powder material that forms;
(2), in the mode while the glue spraying of feeding in raw material, yttrium stable zirconium oxide powder and epoxy glue are joined in the coater, the inboard wall of cylinder block of coater is coated with the uniform polyurethane coating of a layer thickness, generate zirconia ceramics microballon green compact by the rolling moulding, wherein epoxy glue is formulated by PVA, paraffin, CMC, oleic acid and deionized water, and the summation of PVA, paraffin, CMC, oleic acid and the weight ratio of deionized water are 0.01:1;
The rolling moulding generates zirconia ceramics microballon green compact and comprises generation zirconia ceramics microballon kind substep and generate zirconia ceramics microballon green compact step;
Generating zirconia ceramics microballon kind substep comprises:
(2-1-1), start coater, the rotating speed of coater is controlled at 15 rev/mins (in scopes of 15～45 rev/mins can);
(2-1-2), the yttrium stable zirconium oxide powder is disperseed simultaneously, slowly to add epoxy glue in the coater by spray gun in the adding coater;
(2-1-3), the moulding of in coater, rolling, be the zirconia ceramics microballon seed that 0.02mm is above and have higher hardness until generate diameter, then take out;
Generating zirconia ceramics microballon green compact step comprises:
(2-2-1), start coater, the rotating speed of coater is controlled at 15 rev/mins (in scopes of 15～45 rev/mins can);
(2-2-2), with disposable the joining in the coater of zirconia ceramics microballon seed that step (2-1-3) generates, simultaneously, slowly add epoxy glue in the coater by spray gun;
(2-2-3), in the rolling moulding process, adopt diverting device that the zirconia ceramics microballon seed that is stained with epoxy glue is disperseed;
(2-2-4), after zirconia ceramics microballon seed disperses, in coater, disperse to add the yttrium stable zirconium oxide powder, continue the rolling moulding, until zirconia ceramics microballon seed is with bonding solid with the yttrium stable zirconium oxide powder;
(2-2-5), by spray gun epoxy glue is slowly added in the coater, then continue performing step (2-2-3), (2-2-4), until the diameter of the zirconia ceramics microballon green compact that generate reaches till the requirement;
(3), with the insulation 3 hours under the temperature of 1400 ℃ (in scopes of 1400 ℃～1550 ℃ can) of zirconia ceramics microballon green compact (in 3～6 hours the scope can), sinter zirconia ceramics microballon blank into;
(4), adopt the aluminum oxide radioceramic as polishing medium, zirconia ceramics microballon blank is polished, obtain finished product zirconia ceramics microballon.
Above-mentioned diverting device comprises support 1, tilting mechanism 2, connecting rod 3, swing seat 4, soft 5 in many plastics, elevating bracket 6 and arrangement for adjusting height 7, and the dual-side that plastics are soft 5 is spline-simulating; Elevating bracket 6 is installed on the support 1 and can slides along the vertical direction on support 1, and arrangement for adjusting height 7 is installed on the support 1, and the clutch end of arrangement for adjusting height 7 is connected with elevating bracket 6, and tilting mechanism 2 is installed on the elevating bracket 6; One end of connecting rod 3 is connected with the clutch end of tilting mechanism 2, and the other end of connecting rod 3 is connected with swing seat 4; Soft 5 in plastics are installed on the swing seat 4.
Arrangement for adjusting height 7 comprises mounting block 701 and screw rod 702, mounting block 701 is installed on the support 1, offer through hole 703 along the vertical direction on the mounting block 1, offer screw 704 along the vertical direction on the elevating bracket 6, screw rod 702 is in through hole 703 and the screw 704, makes elevating bracket 6 rise or descend by turning screw rod 702, regulates at any time the height of elevating bracket 6, thereby the height that the adjusting plastics are soft 5, it is quite convenient to operate.
In other embodiment of the present embodiment, the yttrium stable zirconium oxide powder is by 5.5% Y
20
3With 94.5% Zr(Hf) O
2The compound zirconium powder material that forms.
In other embodiment of the present embodiment, the yttrium stable zirconium oxide powder is by 5% Y
20
3With 95% Zr(Hf) O
2The compound zirconium powder material that forms.
In other embodiment of the present embodiment, epoxy glue is formulated by PVA, paraffin, CMC, oleic acid and deionized water, and the summation of PVA, paraffin, CMC, oleic acid and the weight ratio of deionized water are 0.02:1.
Embodiment example two
In the situation that other parts are all identical with embodiment one, its difference is: adopt the cerium stabilizing zirconium oxide powder to replace the yttrium stable zirconium oxide powder, the cerium stabilizing zirconium oxide powder is by 6% CeO
2With 94% Zr(Hf) O
2The compound zirconium powder material that forms.
In other embodiment of the present embodiment, the cerium stabilizing zirconium oxide powder is by 20% CeO
2With 80% Zr(Hf) O
2The compound zirconium powder material that forms.
In other embodiment of the present embodiment, the cerium stabilizing zirconium oxide powder is by 12% CeO
2With 88% Zr(Hf) O
2The compound zirconium powder material that forms.
In addition; need to prove, the specific embodiment described in this specification sheets, its each several part titles etc. can be different; allly conceive equivalence or the simple change that described structure, feature and principle are done according to patent of the present invention, be included in the protection domain of patent of the present invention.Those skilled in the art can make various modifications or replenish or adopt similar mode to substitute described specific embodiment; only otherwise depart from structure of the present invention or surmount this scope as defined in the claims, all should belong to protection scope of the present invention.
Claims (10)
1. the moulding of rolling prepares the method for zirconia ceramics microballon, it is characterized in that comprising the steps:
(1), yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder is disperseed;
(2), in the mode while the glue spraying of feeding in raw material, yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder and epoxy glue are joined in the coater, generate zirconia ceramics microballon green compact by the rolling moulding;
(3), zirconia ceramics microballon green compact are incubated 3～6 hours under 1400 ℃～1550 ℃ temperature, sinter zirconia ceramics microballon blank into;
(4), zirconia ceramics microballon blank is polished, obtain finished product zirconia ceramics microballon.
2. rolling moulding as claimed in claim 1 prepares the method for zirconia ceramics microballon, it is characterized in that: described yttrium stable zirconium oxide powder is by Y
20
3And Zr(Hf) O
2The compound zirconium powder material that forms, each compositions in weight percentage is: Y
20
34.9～5.5%, Zr(Hf) O
294.5～95.1%; Described cerium stabilizing zirconium oxide powder is by CeO
2And Zr(Hf) O
2The compound zirconium powder material that forms, each compositions in weight percentage is: CeO
26～20%, Zr(Hf) O
280～94%.
3. rolling moulding as claimed in claim 1 prepares the method for zirconia ceramics microballon, it is characterized in that: described epoxy glue is formulated by PVA, paraffin, CMC, oleic acid and deionized water, and the summation of PVA, paraffin, CMC, oleic acid and the weight ratio of deionized water are (0.01～0.02): 1.
4. each described rolling moulding prepares the method for zirconia ceramics microballon such as claim 1～3, it is characterized in that: described yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder is by the preparation of ball milling granulation process.
5. each described rolling moulding prepares the method for zirconia ceramics microballon such as claim 1～3, it is characterized in that: described yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder disperses by micronizer mill, the pressure of micronizer mill is equal to or greater than 1.0Mpa, reinforced air pressure is 0.2～1.0Mpa, and feed rate is 0.05～0.5 kg/minute.
6. each described rolling moulding prepares the method for zirconia ceramics microballon such as claim 1～3, it is characterized in that: described step (2) specifically comprises and generates zirconia ceramics microballon kind substep and generate zirconia ceramics microballon green compact step;
Generating zirconia ceramics microballon kind substep comprises:
(2-1-1), start coater, the rotating speed of coater is controlled at 15～45 rev/mins;
(2-1-2), yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder is disperseed simultaneously, slowly to add epoxy glue in the coater by spray gun in the adding coater;
(2-1-3), the moulding of in coater, rolling, be the zirconia ceramics microballon seed that 0.02mm is above and have higher hardness until generate diameter, then take out;
Generating zirconia ceramics microballon green compact step comprises:
(2-2-1), start coater, the rotating speed of coater is controlled at 15～45 rev/mins;
(2-2-2), with disposable the joining in the coater of zirconia ceramics microballon seed that step (2-1-3) generates, simultaneously, slowly add epoxy glue in the coater by spray gun;
(2-2-3), in the rolling moulding process, adopt diverting device that the zirconia ceramics microballon seed that is stained with epoxy glue is disperseed;
(2-2-4), after zirconia ceramics microballon seed disperses, in coater, disperse to add yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder, continue the rolling moulding, until zirconia ceramics microballon seed is with bonding solid with yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder;
(2-2-5), by spray gun epoxy glue is slowly added in the coater, then continue performing step (2-2-3), (2-2-4), until the diameter of the zirconia ceramics microballon green compact that generate reaches till the requirement.
7. rolling moulding as claimed in claim 6 prepares the method for zirconia ceramics microballon, it is characterized in that: described diverting device comprises support, draws together tilting mechanism, connecting rod, swing seat, soft of many plastics, elevating bracket and arrangement for adjusting height; Elevating bracket is rack-mount and can be on support slide along the vertical direction, and arrangement for adjusting height is rack-mount, and the clutch end of arrangement for adjusting height is connected with elevating bracket, and tilting mechanism is installed on the elevating bracket; One end of connecting rod is connected with the clutch end of tilting mechanism, and the other end of connecting rod is connected with swing seat; Soft of plastics are installed on the swing seat.
8. rolling moulding as claimed in claim 7 prepares the method for zirconia ceramics microballon, and it is characterized in that: the dual-side that described plastics are soft is spline-simulating.
9. rolling moulding as claimed in claim 1 prepares the method for zirconia ceramics microballon, it is characterized in that: the inboard wall of cylinder block of described coater is coated with the uniform polyurethane coating of a layer thickness.
10. rolling moulding as claimed in claim 1 prepares the method for zirconia ceramics microballon, it is characterized in that: adopt the aluminum oxide radioceramic to polish as polishing medium.
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| CN107573064A (en) * | 2017-10-11 | 2018-01-12 | 东莞市日进德新材料技术有限公司 | Zirconia ceramics microballon and preparation method thereof |
| CN110451962A (en) * | 2019-08-23 | 2019-11-15 | 内蒙古科技大学 | A kind of submillimeter level zirconia ceramics ball and preparation method thereof |
| CN111233486A (en) * | 2020-02-24 | 2020-06-05 | 长裕控股集团有限公司 | Preparation method of ceramic microspheres |
| CN111233486B (en) * | 2020-02-24 | 2023-05-05 | 长裕控股集团股份有限公司 | Preparation method of ceramic microbeads |
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