CN106830927A - The method that a kind of shaping of drop shallow lake prepares zirconia ceramics microballon - Google Patents
The method that a kind of shaping of drop shallow lake prepares zirconia ceramics microballon Download PDFInfo
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- CN106830927A CN106830927A CN201710057229.2A CN201710057229A CN106830927A CN 106830927 A CN106830927 A CN 106830927A CN 201710057229 A CN201710057229 A CN 201710057229A CN 106830927 A CN106830927 A CN 106830927A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The method that a kind of shaping of drop shallow lake prepares zirconia ceramics microballon, comprises the following steps:(1)After zirconia ceramics powder is well mixed with epoxy glue, it is added in drop shallow lake former, the preforming formation zirconia ceramics particle of titration is first passed through, the zirconia ceramics particle of formation by gravity by after air-cooling moulding, falling into coolant and collecting and formed zirconia ceramics microballon green compact;(2)The zirconia ceramics microballon green compact that will be collected into take out from coolant, are then placed in being heated to 40~90 DEG C in degreaser carrying out degreasing;(3)The zirconia ceramics microballon green compact for completing degreasing are incubated 3~6 hours at a temperature of 1350~1550 DEG C, zirconia ceramics microballon blank is sintered into;(4)Zirconia ceramics microballon blank is polished, zirconia ceramics microballon is obtained.Using the zirconia ceramics microballon method of the invention, it is possible to prepared small dimension, the zirconia ceramics microballon being made is more uniform, more wear-resisting.
Description
Technical field
The present invention relates to ceramic material manufacture method, and in particular to a kind of shaping of drop shallow lake prepares the side of zirconia ceramics microballon
Method.
Background technology
As superfine powder demand is more and more vigorous, the demand for the abrasive media of the following specifications of particle diameter 1mm is also more next
It is bigger.Wear-resisting, the corrosion-resistant, resistance to elevated temperatures that zirconia ceramics abrasive media possesses because of it, and it is widely used in grinding
Dispersion industry, however, existing preparation technology is difficult to meet the requirement of its anti-wear performance and/or dimensions, therefore compels to be essential
Small dimension zirconia ceramics abrasive media relatively more resistant to abrasive wear is prepared with a kind of new technology.
The content of the invention
The technical problem to be solved in the present invention is to provide the method that a kind of shaping of drop shallow lake prepares zirconia ceramics microballon, this
The method that drop shallow lake shaping prepares zirconia ceramics microballon can produce more resistant zirconia ceramics microballon.The technical side of use
Case is as follows:
The method that a kind of shaping of drop shallow lake prepares zirconia ceramics microballon, it is characterised in that comprise the following steps:
(1)Drop is formed sediment and is molded
After zirconia ceramics powder is well mixed with epoxy glue, it is added in drop shallow lake former, first passes through titration preforming
Zirconia ceramics particle is formed, the zirconia ceramics particle of formation by gravity by after air-cooling moulding, falling into coolant and receiving
Collect and formed zirconia ceramics microballon green compact;
(2)Degreasing
The zirconia ceramics microballon green compact that will be collected into take out from coolant, are then placed in being heated to 40~90 DEG C in degreaser
Carry out degreasing;
(3)Heat preservation sintering
The zirconia ceramics microballon green compact for completing degreasing are incubated 3~6 hours at a temperature of 1350~1550 DEG C, oxygen is sintered into
Change zircon ceramic microballon blank;
(4)Polishing
Zirconia ceramics microballon blank is polished, zirconia ceramics microballon is obtained.
In preferred scheme, above-mentioned zirconia ceramics powder is yttrium stable zirconium oxide powder or cerium stabilizing zirconium oxide powder.It is a kind of excellent
In selecting scheme, above-mentioned yttrium stable zirconium oxide powder by 4.9~5.5% (weight) Y203With the Zr (Hf) of 94.5~95.1% (weight)
O2Composition.In another preferred scheme, above-mentioned cerium stabilizing zirconium oxide powder by 6~20% (weight) CeO2With 80~94% (weight)
Zr (Hf) O2Composition.Above-mentioned Zr (Hf) O2It is zirconium oxide, hafnium oxide by 1:1 molar ratio formed with stablizing lattice
Oxide.
In preferred scheme, above-mentioned zirconia ceramics powder(Such as yttrium stable zirconium oxide powder or cerium stabilizing zirconium oxide powder)By ball
It is prepared by mill prilling.Ball milling prilling is mainly by ball mill to produce powder, the zirconia ceramics powder being thus made
The characteristics of material has epigranular.
Preferred steps(1)In, before above-mentioned zirconia ceramics powder mixes with epoxy glue, first zirconia ceramics powder is entered
The treatment of row sign.Sign treatment is that zirconia ceramics powder is heat-treated in middle temperature kiln first, then in milling apparatus
In granularity homogenizing treatment is carried out to zirconia ceramics powder, zirconia ceramics powder is carried out at dispersion in dispersing apparatus finally
The process of reason.The purpose for characterizing treatment is to reach on microcosmic uniform, macroscopically meets the graininess that drop is formed sediment required for shaping
Process.
More preferably in scheme, it is to the method that zirconia ceramics powder carries out decentralized processing in dispersing apparatus:By gas
Stream pulverizer disperses to zirconia ceramics powder, and the pressure of airslide disintegrating mill is equal to or more than 1.0Mpa, and charging air pressure is
0.2~1.0Mpa, charging rate is 0.05~0.5 kg/min.Using airslide disintegrating mill to zirconia ceramics powder(Such as yttrium
Stabilizing zirconia powder or cerium stabilizing zirconium oxide powder)Disperseed, all particles can be almost completely dispersed and come, be conducive to carrying
High yield quality and yield rate.
Step(1)In, the process of drop shallow lake shaping is:First the mixed material of zirconia ceramics powder and epoxy glue will be heated into
It is feed liquid, by the surface tension of liquid, is first titrated by pressure and self gravitation and be pre-formed as zirconia ceramics particle(Oxidation
Zircon ceramic particle is generally spherical in shape);Zirconia ceramics particle through air-cooling moulding, finally sinks in the collecting tank for have coolant again
Form sediment and shape.Zirconia ceramics particle during coolant is fallen into by gravity, and air contact, so as to by air-cooling moulding.
In preferred scheme, above-mentioned epoxy glue is by polyvinyl alcohol(PVA), paraffin and oleic acid is formulated.Using PVA, paraffin
The epoxy glue being configured to oleic acid, its viscosity is high, is adapted to the bonding of yttrium stable zirconium oxide powder/cerium stabilizing zirconium oxide powder, after bonding
It is quite firm.More preferably above-mentioned epoxy glue by the polyvinyl alcohol of 0.1-15% (weight), the paraffin of 84.9-99.5% (weight) and
The oleic acid composition of 0.1-5% (weight).
In preferred scheme, step(1)Middle zirconia ceramics powder is with the part by weight of epoxy glue(60~90):(10~
40).
It is preferred that above-mentioned coolant is made up of kerosene, oleic acid and blender.More preferably above-mentioned coolant is by 75-95% (weight)
Kerosene, the oleic acid of 0.6-10% (weight) and 1-15% (weight) blender composition.Above-mentioned blender can be that density is
The oily substance of 0.6-1.2g/cm3, for adjusting the density and viscosity of coolant, preferably above-mentioned blender be gasoline, heavy oil,
Diesel oil and vegetable oil(Such as corn oil, rapeseed oil, cottonseed oil, linseed oil, peanut oil etc.)In one kind or many of
Combination.
In preferred scheme, above-mentioned steps(1)The step of generation zirconia ceramics microballon green compact, includes:
(1-1)Polyvinyl alcohol, paraffin and oleic acid are mixed and heated to 60~150 DEG C, stirring is mixed to well mixed
Glue;
(1-2)Zirconia ceramics powder and epoxy glue are added in the banbury with froth in vacuum function, at 60~150 DEG C
Lower banburying 1.5~5 hours, the mixed material to zirconia ceramics powder and epoxy glue while banburying carries out froth in vacuum;
(1-3)By step(1-2)Mixed material obtained by banburying is added in drop shallow lake former, and 60~150 are heated to after sealing
DEG C and be incubated, vacuum be homogenized 0~2 hour;Then by titrating preforming formation zirconia ceramics particle(In titration process, root
According to the amount of storage regulation drop shallow lake former air pressure inside of mixed material, it is ensured that air pressure inside adds mixed material self gravitation just
Stably ooze);
(1-4)Step(1-3)The zirconia ceramics particle of gained relies on gravity fall, and zirconia ceramics particle is in the process for falling
It is middle by air-cooling moulding, fallen into coolant after the height of 20~70cm of zirconia ceramics particles fall collect and formed zirconium oxide pottery
Porcelain microballon green compact.
Step(1-3)The diameter of the zirconia ceramics particle for obtaining usually 0.001-1mm, it is substantially spherical in shape.
Step(2)Middle degreasing refers to remove the epoxy glue in zirconia ceramics microballon green compact.It is preferred that degreasing time is that 1-4 is small
When.
In preferred scheme, above-mentioned drop shallow lake former includes support, charging basket, vacuum homogenizing device, thermostatic control system, perseverance
Pressure control system(The constant pressure of constant-voltage system is realized by filling inert gas)And tank level control system, charging basket be provided with charge door and
Discharging opening.In the forming process of zirconia ceramics microballon green compact, vacuum homogenizing device be mixed material add charging basket in after,
Vacuum before mixed material to adding is molded is homogenized, and prevents the residual of bubble;Thermostatic control system and Isobarically Control system
System is for ensureing the uniformity of shaping, and wherein thermostatic control system ensures that the mobility of mixed material is consistent, Isobarically Control
System ensures the uniformity of discharging opening mixed material stress;Tank level control system is for mixed material liquid level is too high in preventing charging basket
Or too low generation substandard product.Using this drop shallow lake former, because epoxy glue is fully mixed with zirconia ceramics powder
Close, and there is vacuum to be homogenized, ensured the uniformity of mixed material;Using thermostatic control system, control system of invariable pressure, Liquid level
System is ensureing the uniformity of discharging;By the sphericity for adjusting the surface tension of liquid to ensure product.Therefore, using this
Drop shallow lake former carries out drop and forms sediment shaping, can ensure the equal of spheroid on microcosmic in the production process of zirconia ceramics microballon
Even property, raising balling-up speed, raising ball-formation quality.
The present invention carries out sign treatment by zirconia ceramics powder, zirconia ceramics powder is filled with epoxy glue
Point mix and be mingled with without other, then pass through to drip the method for shaping of forming sediment and generate zirconia ceramics microballon green compact, then 1350~
Heat preservation sintering at a temperature of 1550 DEG C, is finally processed by shot blasting, the zirconia ceramics microballon being made is more uniform, more resistance to
Mill.Using the zirconia ceramics microballon method of the invention, it is possible to prepared small dimension, its diameter is usually 0.001~1mm.
Brief description of the drawings
Fig. 1 is the structural representation of drop shallow lake former used in the preferred embodiment of the present invention.
Specific embodiment
Embodiment 1
The method that the drop shallow lake shaping of the present embodiment prepares zirconia ceramics microballon comprises the following steps:
(1)Drop is formed sediment and is molded
After zirconia ceramics powder is well mixed with epoxy glue, it is added in drop shallow lake former, first passes through titration preforming
Zirconia ceramics particle is formed, the zirconia ceramics particle of formation by gravity by after air-cooling moulding, falling into coolant and receiving
Collect and formed zirconia ceramics microballon green compact;
(2)Degreasing
The zirconia ceramics microballon green compact that will be collected into take out from coolant, are then placed in being heated to 80 DEG C in degreaser carrying out
Degreasing, degreasing time is 2 hours;
(3)Heat preservation sintering
The zirconia ceramics microballon green compact for completing degreasing are incubated 4 hours at a temperature of 1400 DEG C, zirconia ceramics is sintered into
Microballon blank;
(4)Polishing
Zirconia ceramics microballon blank is polished, zirconia ceramics microballon is obtained.
Step(1)In, before zirconia ceramics powder mixes with epoxy glue, first zirconia ceramics powder is carried out at sign
Reason, sign treatment is that zirconia ceramics powder is heat-treated in middle temperature kiln first, then to oxidation in milling apparatus
Zircon ceramic powder carries out granularity homogenizing treatment, finally carries out the mistake of decentralized processing to zirconia ceramics powder in dispersing apparatus
Journey.It is to the method that zirconia ceramics powder carries out decentralized processing in dispersing apparatus:Zirconium oxide is made pottery by airslide disintegrating mill
Ceramic powder is disperseed, and the pressure of airslide disintegrating mill is 1.1Mpa, and charging air pressure is 0.5Mpa, and charging rate is 0.2 thousand Grams Per Minutes
Clock.
In the present embodiment, step(1)The step of generation zirconia ceramics microballon green compact, specifically includes:
(1-1)By polyvinyl alcohol, paraffin and oleic acid(By weight, the ratio of polyvinyl alcohol, paraffin and oleic acid is polyvinyl alcohol
8%th, paraffin 89%, oleic acid 3%)100 DEG C are mixed and heated to, stirring obtains epoxy glue to well mixed(The epoxy glue for obtaining by
The oleic acid composition of the polyvinyl alcohol of 8% (weight), the paraffin of 89% (weight) and 3% (weight));
(1-2)Zirconia ceramics powder and epoxy glue are added in the banbury with froth in vacuum function, it is close at 100 DEG C
Refining 3.5 hours, the mixed material to zirconia ceramics powder and epoxy glue while banburying carries out froth in vacuum;
Above-mentioned zirconia ceramics powder is by 4.9% Y203Zr with 95.1%(Hf)O2The yttrium stable zirconium oxide powder for being constituted;Oxygen
It is 80 to change zircon ceramic powder with the part by weight of epoxy glue:20;
(1-3)By step(1-2)Mixed material obtained by banburying is added in drop shallow lake former, and 100 DEG C are heated to after sealing simultaneously
Insulation, vacuum is homogenized 1 hour;Then by titrating preforming formation zirconia ceramics particle(In titration process, according to mixture
The amount of storage regulation drop shallow lake former air pressure inside of material, it is ensured that air pressure inside adds mixed material self gravitation just stably to drip
Go out);
(1-4)Step(1-3)The zirconia ceramics particle of gained relies on gravity fall, and zirconia ceramics particle is in the process for falling
It is middle by air-cooling moulding, fallen into coolant after the height of zirconia ceramics particles fall 50cm and collected and to form zirconia ceramics micro-
Pearl green compact.
Above-mentioned coolant by 85% (weight) kerosene, the oleic acid of 7% (weight) and 8% (weight) blender(It is vapour
Oil)Composition.
Press《JC/T2136-2012 crystallite zirconia abrasive media balls》The zirconium oxide that the method for testing test of appendix A is obtained
The abrasion of ceramic fine bead, it is 0.011g/ to wear away(kg·h).
Embodiment 2
The method that the drop shallow lake shaping of the present embodiment prepares zirconia ceramics microballon comprises the following steps:
(1)Drop is formed sediment and is molded
After zirconia ceramics powder is well mixed with epoxy glue, it is added in drop shallow lake former, first passes through titration preforming
Zirconia ceramics particle is formed, the zirconia ceramics particle of formation by gravity by after air-cooling moulding, falling into coolant and receiving
Collect and formed zirconia ceramics microballon green compact;
(2)Degreasing
The zirconia ceramics microballon green compact that will be collected into take out from coolant, are then placed in being heated to 90 DEG C in degreaser carrying out
Degreasing, degreasing time is 1 hour;
(3)Heat preservation sintering
The zirconia ceramics microballon green compact for completing degreasing are incubated 6 hours at a temperature of 1350 DEG C, zirconia ceramics is sintered into
Microballon blank;
(4)Polishing
Zirconia ceramics microballon blank is polished, zirconia ceramics microballon is obtained.
Step(1)In, before zirconia ceramics powder mixes with epoxy glue, first zirconia ceramics powder is carried out at sign
Reason, sign treatment is that zirconia ceramics powder is heat-treated in middle temperature kiln first, then to oxidation in milling apparatus
Zircon ceramic powder carries out granularity homogenizing treatment, finally carries out the mistake of decentralized processing to zirconia ceramics powder in dispersing apparatus
Journey.It is to the method that zirconia ceramics powder carries out decentralized processing in dispersing apparatus:Zirconium oxide is made pottery by airslide disintegrating mill
Ceramic powder is disperseed, and the pressure of airslide disintegrating mill is 1.0Mpa, and charging air pressure is 1.0Mpa, and charging rate is 0.5 thousand Grams Per Minutes
Clock.
In the present embodiment, step(1)The step of generation zirconia ceramics microballon green compact, specifically includes:
(1-1)By polyvinyl alcohol, paraffin and oleic acid(By weight, the ratio of polyvinyl alcohol, paraffin and oleic acid is polyvinyl alcohol
15%th, paraffin 84.9%, oleic acid 0.1%)60 DEG C are mixed and heated to, stirring obtains epoxy glue to well mixed(The mixing for obtaining
Glue is made up of the oleic acid of the polyvinyl alcohol, the paraffin of 84.9% (weight) and 0.1% (weight) of 15% (weight));
(1-2)Zirconia ceramics powder and epoxy glue are added in the banbury with froth in vacuum function, it is close at 150 DEG C
Refining 1.5 hours, the mixed material to zirconia ceramics powder and epoxy glue while banburying carries out froth in vacuum;
Above-mentioned zirconia ceramics powder is by 5.5% Y203Zr with 94.5%(Hf)O2The yttrium stable zirconium oxide powder for being constituted;Oxygen
It is 60 to change zircon ceramic powder with the part by weight of epoxy glue:40;
(1-3)By step(1-2)Mixed material obtained by banburying is added in drop shallow lake former, and 150 DEG C are heated to after sealing simultaneously
Insulation, vacuum is homogenized 0.1 hour;Then by titrating preforming formation zirconia ceramics particle(In titration process, according to mixing
The amount of storage regulation drop shallow lake former air pressure inside of material, it is ensured that air pressure inside adds mixed material self gravitation just stably
Ooze);
(1-4)Step(1-3)The zirconia ceramics particle of gained relies on gravity fall, and zirconia ceramics particle is in the process for falling
It is middle by air-cooling moulding, fallen into coolant after the height of zirconia ceramics particles fall 70cm and collected and to form zirconia ceramics micro-
Pearl green compact.
Above-mentioned coolant by 95% (weight) kerosene, the oleic acid of 4% (weight) and 1% (weight) blender(The blender
It is made up of heavy oil and diesel oil, wherein heavy oil and diesel oil respectively accounts for half)Composition.
Press《JC/T2136-2012 crystallite zirconia abrasive media balls》The zirconium oxide that the method for testing test of appendix A is obtained
The abrasion of ceramic fine bead, it is 0.014g/ to wear away(kg·h).
Embodiment 3
The method that the drop shallow lake shaping of the present embodiment prepares zirconia ceramics microballon comprises the following steps:
(1)Drop is formed sediment and is molded
After zirconia ceramics powder is well mixed with epoxy glue, it is added in drop shallow lake former, first passes through titration preforming
Zirconia ceramics particle is formed, the zirconia ceramics particle of formation by gravity by after air-cooling moulding, falling into coolant and receiving
Collect and formed zirconia ceramics microballon green compact;
(2)Degreasing
The zirconia ceramics microballon green compact that will be collected into take out from coolant, are then placed in being heated to 40 DEG C in degreaser carrying out
Degreasing, degreasing time is 4 hours;
(3)Heat preservation sintering
The zirconia ceramics microballon green compact for completing degreasing are incubated 3 hours at a temperature of 1550 DEG C, zirconia ceramics is sintered into
Microballon blank;
(4)Polishing
Zirconia ceramics microballon blank is polished, zirconia ceramics microballon is obtained.
Step(1)In, before zirconia ceramics powder mixes with epoxy glue, first zirconia ceramics powder is carried out at sign
Reason, sign treatment is that zirconia ceramics powder is heat-treated in middle temperature kiln first, then to oxidation in milling apparatus
Zircon ceramic powder carries out granularity homogenizing treatment, finally carries out the mistake of decentralized processing to zirconia ceramics powder in dispersing apparatus
Journey.It is to the method that zirconia ceramics powder carries out decentralized processing in dispersing apparatus:Zirconium oxide is made pottery by airslide disintegrating mill
Ceramic powder is disperseed, and the pressure of airslide disintegrating mill is 1.2Mpa, and charging air pressure is 0.2Mpa, charging rate for 0.05 kilogram/
Minute.
In the present embodiment, step(1)The step of generation zirconia ceramics microballon green compact, specifically includes:
(1-1)By polyvinyl alcohol, paraffin and oleic acid(By weight, the ratio of polyvinyl alcohol, paraffin and oleic acid is polyvinyl alcohol
0.1%th, paraffin 99%, oleic acid 0.9%)150 DEG C are mixed and heated to, stirring obtains epoxy glue to well mixed(The mixing for obtaining
Glue is made up of the oleic acid of the polyvinyl alcohol, the paraffin of 99% (weight) and 0.9% (weight) of 0.1% (weight));
(1-2)Zirconia ceramics powder and epoxy glue are added in the banbury with froth in vacuum function, it is close at 60 DEG C
Refining 5 hours, the mixed material to zirconia ceramics powder and epoxy glue while banburying carries out froth in vacuum;
Above-mentioned zirconia ceramics powder is by 5% Y203Zr with 95%(Hf)O2The yttrium stable zirconium oxide powder for being constituted;Zirconium oxide
Ceramic powder is 90 with the part by weight of epoxy glue:10;
(1-3)By step(1-2)Mixed material obtained by banburying is added in drop shallow lake former, 60 DEG C is heated to after sealing and is protected
Temperature, vacuum is homogenized 2 hours;Then by titrating preforming formation zirconia ceramics particle(In titration process, according to mixed material
Amount of storage regulation drop shallow lake former air pressure inside, it is ensured that air pressure inside adds mixed material self gravitation just stably to drip
Go out);
(1-4)Step(1-3)The zirconia ceramics particle of gained relies on gravity fall, and zirconia ceramics particle is in the process for falling
It is middle by air-cooling moulding, fallen into coolant after the height of zirconia ceramics particles fall 30cm and collected and to form zirconia ceramics micro-
Pearl green compact.
Above-mentioned coolant by 75% (weight) kerosene, the oleic acid of 10% (weight) and 15% (weight) blender(It is jade
Rice bran oil)Composition.
Press《JC/T2136-2012 crystallite zirconia abrasive media balls》The zirconium oxide that the method for testing test of appendix A is obtained
The abrasion of ceramic fine bead, it is 0.012g/ to wear away(kg·h).
Embodiment 4
The present embodiment is with the difference of embodiment 1:Yttrium stable zirconium oxide powder, cerium Stable Oxygen are replaced using cerium stabilizing zirconium oxide powder
Change CeO of the zirconium powder by 6% (weight)2With the Zr of 94% (weight)(Hf)O2Composition.
The present embodiment remainder is same as Example 1.
Press《JC/T2136-2012 crystallite zirconia abrasive media balls》The zirconium oxide that the method for testing test of appendix A is obtained
The abrasion of ceramic fine bead, it is 0.011g/ to wear away(kg·h).
Embodiment 5
The present embodiment is with the difference of embodiment 2:Yttrium stable zirconium oxide powder, cerium Stable Oxygen are replaced using cerium stabilizing zirconium oxide powder
Change CeO of the zirconium powder by 20% (weight)2With the Zr of 80% (weight)(Hf)O2Composition.
The present embodiment remainder is same as Example 1.
Press《JC/T2136-2012 crystallite zirconia abrasive media balls》The zirconium oxide that the method for testing test of appendix A is obtained
The abrasion of ceramic fine bead, it is 0.010g/ to wear away(kg·h).
Embodiment 6
The present embodiment is with the difference of embodiment 3:Yttrium stable zirconium oxide powder, cerium Stable Oxygen are replaced using cerium stabilizing zirconium oxide powder
Change CeO of the zirconium powder by 12% (weight)2With the Zr of 88% (weight)(Hf)O2Composition.
The present embodiment remainder is same as Example 1.
Press《JC/T2136-2012 crystallite zirconia abrasive media balls》The zirconium oxide that the method for testing test of appendix A is obtained
The abrasion of ceramic fine bead, it is 0.011g/ to wear away(kg·h).
Drop shallow lake former used by embodiment 1-6 can use conventional equipment.For example, the drop shallow lake former shown in Fig. 1 includes
Support, charging basket 1, vacuum homogenizing device(Not shown in Fig. 1), thermostatic control system, control system of invariable pressure and tank level control system,
Charging basket 1 is provided with a charge door 11 and multiple discharging openings 12, and, located at the top of charging basket 1, each discharging opening 12 is located at material for charge door 11
1 bottom of bucket.In the forming process of zirconia ceramics microballon green compact, vacuum homogenizing device mixed material add charging basket 1 in after,
Vacuum before mixed material to adding is molded is homogenized, and prevents the residual of bubble.Thermostatic control system ensures mixed material
Mobility it is consistent, control system of invariable pressure ensures the uniformity of discharging opening mixed material stress;Tank level control system is to prevent
The too high or too low generation substandard product of mixed material liquid level in charging basket.Above-mentioned thermostatic control system, control system of invariable pressure and liquid
Level controlling system by it is following control circuits 2, temperature sensor 3, heater 4, pressure sensor 5, air accumulator 6, air inlet pipe 7,
Choke valve 8 and liquid level sensor 9 are constituted, temperature sensor 3, pressure sensor 5, temperature sensor 9 respectively with control the phase of circuit 2
The input answered is connected, and choke valve 8 and the corresponding output end of control circuit 2 are connected, temperature sensor 3, pressure sensor 5, temperature
Degree sensor 9 is in charging basket 1(Wherein pressure sensor 5 is in the bottom of charging basket 1), heater 4 located at the outside of charging basket 1,
The air inlet of air inlet pipe 7 is connected with air accumulator 6, and the gas outlet of air inlet pipe 7 is in charging basket 1, and choke valve 8 is in air inlet pipe 7.
Temperature sensor 3 detects the temperature of charge in charging basket 1 and sends to control circuit 2 temperature signal that control circuit 2 is sent out after processing
Control signal to heater 4 is sent, the heating power to heater 4 is adjusted, the temperature of charge in charging basket 1 is kept steady
It is fixed, realize thermostatic control.Storing liquid inert gas in air accumulator 6, through air inlet pipe 7 to inert gas is filled in charging basket 1, in material
Air pressure is produced in bucket 1;Pressure of detection charging basket 1 bottom of pressure sensor 5 at discharging opening 12, and by pressure signal send to
Control circuit 2, control circuit 2 sends a control signal to choke valve 8 after processing, and the air inflow to air inlet pipe 7 is adjusted, so that
The size of air pressure in regulation charging basket 1, makes pressure remained steady of the bottom of charging basket 1 at discharging opening 12, realizes Isobarically Control.Liquid
Material liquid level in the detection charging basket 1 of level sensor 9 is simultaneously sent to control circuit 2, when detecting material liquid level mistake liquid level signal
Control circuit 2 to send cue when high or too low, charging is reminded when material liquid level is too low, reminded when material liquid level is too high and stopped
Charging, realizes Liquid level.
Claims (10)
1. the method that a kind of shaping of drop shallow lake prepares zirconia ceramics microballon, it is characterised in that comprise the following steps:
(1)Drop is formed sediment and is molded
After zirconia ceramics powder is well mixed with epoxy glue, it is added in drop shallow lake former, first passes through titration preforming
Zirconia ceramics particle is formed, the zirconia ceramics particle of formation by gravity by after air-cooling moulding, falling into coolant and receiving
Collect and formed zirconia ceramics microballon green compact;
(2)Degreasing
The zirconia ceramics microballon green compact that will be collected into take out from coolant, are then placed in being heated to 40~90 DEG C in degreaser
Carry out degreasing;
(3)Heat preservation sintering
The zirconia ceramics microballon green compact for completing degreasing are incubated 3~6 hours at a temperature of 1350~1550 DEG C, oxygen is sintered into
Change zircon ceramic microballon blank;
(4)Polishing
Zirconia ceramics microballon blank is polished, zirconia ceramics microballon is obtained.
2. the method that drop shallow lake according to claim 1 shaping prepares zirconia ceramics microballon, it is characterised in that:The oxidation
Zircon ceramic powder is yttrium stable zirconium oxide powder or cerium stabilizing zirconium oxide powder.
3. the method that drop shallow lake according to claim 2 shaping prepares zirconia ceramics microballon, it is characterised in that:The yttrium is steady
Determine Y of the zirconia powder by 4.9~5.5% (weight)203With Zr (Hf) O of 94.5~95.1% (weight)2Composition.
4. the method that drop shallow lake according to claim 2 shaping prepares zirconia ceramics microballon, it is characterised in that:The cerium is steady
Determine CeO of the zirconia powder by 6~20% (weight)2With Zr (Hf) O of 80~94% (weight)2Composition.
5. the method that drop shallow lake according to claim 1 shaping prepares zirconia ceramics microballon, it is characterised in that:Step(1)
In, before zirconia ceramics powder mixes with epoxy glue, sign treatment first is carried out to zirconia ceramics powder;Sign treatment is first
Zirconia ceramics powder is heat-treated in middle temperature kiln, grain then is carried out to zirconia ceramics powder in milling apparatus
Degree homogenizing treatment, finally carries out the process of decentralized processing in dispersing apparatus to zirconia ceramics powder.
6. the method that drop shallow lake according to claim 5 shaping prepares zirconia ceramics microballon, it is characterised in that:Set in dispersion
It is to the method that zirconia ceramics powder carries out decentralized processing in standby:Zirconia ceramics powder is divided by airslide disintegrating mill
Dissipate, the pressure of airslide disintegrating mill is equal to or more than 1.0Mpa, and charging air pressure is 0.2~1.0Mpa, and charging rate is 0.05~0.5
Kg/min.
7. the method that drop shallow lake according to claim 1 shaping prepares zirconia ceramics microballon, it is characterised in that:The mixing
Glue is made up of the oleic acid of the polyvinyl alcohol, the paraffin of 84.9-99.5% (weight) and 0.1-5% (weight) of 0.1-15% (weight).
8. the method that drop shallow lake according to claim 7 shaping prepares zirconia ceramics microballon, it is characterised in that:Step(1)
The step of generation zirconia ceramics microballon green compact, includes:
(1-1)Polyvinyl alcohol, paraffin and oleic acid are mixed and heated to 60~150 DEG C, stirring is mixed to well mixed
Glue;
(1-2)Zirconia ceramics powder and epoxy glue are added in the banbury with froth in vacuum function, at 60~150 DEG C
Lower banburying 1.5~5 hours, the mixed material to zirconia ceramics powder and epoxy glue while banburying carries out froth in vacuum;
(1-3)By step(1-2)Mixed material obtained by banburying is added in drop shallow lake former, and 60~150 are heated to after sealing
DEG C and be incubated, vacuum be homogenized 0~2 hour;Then by titrating preforming formation zirconia ceramics particle;
(1-4)Step(1-3)The zirconia ceramics particle of gained relies on gravity fall, and zirconia ceramics particle is in the process for falling
It is middle by air-cooling moulding, fallen into coolant after the height of 20~70cm of zirconia ceramics particles fall collect and formed zirconium oxide pottery
Porcelain microballon green compact.
9. the method that the drop shallow lake shaping according to claim any one of 1-8 prepares zirconia ceramics microballon, it is characterised in that:
Step(1)Middle zirconia ceramics powder is with the part by weight of epoxy glue(60~90):(10~40).
10. the method that the drop shallow lake shaping according to claim any one of 1-8 prepares zirconia ceramics microballon, its feature exists
In:The coolant by 75-95% (weight) kerosene, the oleic acid of 0.6-10% (weight) and 1-15% (weight) blender group
Into.
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102584224A (en) * | 2012-02-29 | 2012-07-18 | 重庆利特高新技术有限公司 | Preparation method of nanoscale zirconia ceramic powder for spraying |
CN103319173A (en) * | 2013-06-29 | 2013-09-25 | 广东东方锆业科技股份有限公司 | Method for preparing zirconia ceramic microbead in rolling molding mode |
CN105347832A (en) * | 2015-12-03 | 2016-02-24 | 泉州凯佳新材料研究院有限公司 | Helical carbon fiber composite ceramic for water activation as well as preparation method and application thereof |
US9522848B2 (en) * | 2014-09-04 | 2016-12-20 | Kaohsiung Medical University | Methods for producing a silicon-containing zirconia calcined body and a silicon-containing zirconia sintered body |
-
2017
- 2017-01-26 CN CN201710057229.2A patent/CN106830927B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102584224A (en) * | 2012-02-29 | 2012-07-18 | 重庆利特高新技术有限公司 | Preparation method of nanoscale zirconia ceramic powder for spraying |
CN103319173A (en) * | 2013-06-29 | 2013-09-25 | 广东东方锆业科技股份有限公司 | Method for preparing zirconia ceramic microbead in rolling molding mode |
US9522848B2 (en) * | 2014-09-04 | 2016-12-20 | Kaohsiung Medical University | Methods for producing a silicon-containing zirconia calcined body and a silicon-containing zirconia sintered body |
CN105347832A (en) * | 2015-12-03 | 2016-02-24 | 泉州凯佳新材料研究院有限公司 | Helical carbon fiber composite ceramic for water activation as well as preparation method and application thereof |
Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN108673707A (en) * | 2018-05-10 | 2018-10-19 | 河源帝诺新材料有限公司 | A kind of zirconium oxide microballon high-pressure electrostatic attraction titration former |
CN109761543A (en) * | 2019-03-29 | 2019-05-17 | 深圳市宏通新材料有限公司 | Ceramic microbead production method |
CN110280185A (en) * | 2019-07-09 | 2019-09-27 | 河源帝诺新材料有限公司 | A kind of zirconia grinding media vibration titration moulding process |
CN110423596A (en) * | 2019-08-05 | 2019-11-08 | 河源帝诺新材料有限公司 | A kind of abrasive media titration moulding process |
CN111484351A (en) * | 2019-12-31 | 2020-08-04 | 新兴远建(天津)新材料科技有限公司 | Preparation method and application of lightweight porous ceramic hollow microspheres |
CN111269011A (en) * | 2020-02-18 | 2020-06-12 | 长裕控股集团有限公司 | Preparation method of zirconia microspheres |
CN111269011B (en) * | 2020-02-18 | 2023-05-05 | 长裕控股集团股份有限公司 | Preparation method of zirconia microbeads |
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