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CN105924157A - Preparation method for zirconia ceramic material powder used for preparation of false tooth - Google Patents

Preparation method for zirconia ceramic material powder used for preparation of false tooth Download PDF

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Publication number
CN105924157A
CN105924157A CN201610275449.8A CN201610275449A CN105924157A CN 105924157 A CN105924157 A CN 105924157A CN 201610275449 A CN201610275449 A CN 201610275449A CN 105924157 A CN105924157 A CN 105924157A
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Prior art keywords
zirconia ceramics
material powder
powder body
manufacture method
artificial tooth
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CN201610275449.8A
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Inventor
刘谋山
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Chengdu Besmile Biotechnology Co Ltd
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Chengdu Besmile Biotechnology Co Ltd
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Priority to CN201610275449.8A priority Critical patent/CN105924157A/en
Priority to PCT/CN2016/084126 priority patent/WO2017185469A1/en
Publication of CN105924157A publication Critical patent/CN105924157A/en
Pending legal-status Critical Current

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    • 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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
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    • A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
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Abstract

The invention discloses a preparation method for zirconia ceramic material powder used for preparation of a false tooth. The preparation method comprises the following steps: weighing, preparation of a ceramic precursor, drying and ball milling. The false tooth prepared from the zirconia ceramic material powder provided by the invention has high hardness; and since a dispersing agent is used as a component, the zirconia ceramic material powder overcomes the problems of frangibility, low glossiness, poor color contrast performance and low transparency of an all-ceramic material. The preparation method for the zirconia ceramic material powder is simple and standard to operate, further improves technological parameters of the zirconia ceramic material powder in the process of preparation, improves the utilization rate of a finished product and reduces production cost.

Description

A kind of manufacture method of the zirconia ceramics material powder body made for artificial tooth
Technical field
The invention belongs to bio-medical material and make field, be specifically related to a kind of zirconia ceramics material made for artificial tooth The manufacture method of material powder body.
Background technology
Dispersant (Dispersant) is a kind of to have lipophile and two kinds of opposite nature of hydrophilic in intramolecular simultaneously Interfacial agent.Can homogeneous dispersion those be poorly soluble in liquid inorganic, the solid of organic pigment and liquid particles, the most also Sedimentation and the cohesion of granule can be prevented, form the amphipathic reagent needed for stable suspension.Dispersant can promote gloss, prevent Floating, minimizing flocculation, increase color developing, increase color saturation, increase transparency.
The development of Oral Repair is inseparable with the development of oral cavity material and technique, dentures repai material mainly have pottery, Resin and metal material.And the ceramic material own intensity deficiency of traditional glass ceramics base and alumina base and fragility are relatively big, Easily rupturable, limit its use in the reparation in oral cavity.
Along with developing rapidly of current recovery technique of oral cavity, All-ceramic material is by feat of self good biocompatibility, resistance to A series of speciality such as corrosivity, dielectricity, heat stability and excellent aesthetic effect, become currently used widest oral cavity Repair materials.The All-ceramic material generally making artificial tooth mainly has aluminium oxide and zirconium oxide, and aluminium oxide has good anti-wear performance, But fragility is relatively big, easily rupturable.By contrast zirconium oxide due to other oxides mix effect make it produce stable four directions Crystalline phase, therefore, zirconia ceramics has high tenacity, high-flexural strength and high-wearing feature.Therefore, zirconium oxide is to be currently used for oral cavity The All-ceramic material that in the full magnetic material repaired, mechanical performance is best.But need to carry in hardness and glossiness, color developing etc. Height, is badly in need of the material that exploitation is new.Current zirconia ceramics material powder body manufacture method such as Publication No. CN104528823A Chinese patent disclose a kind of Zirconium powder and preparation method thereof, the manufacture method of Zirconium powder is mentioned by the method But narration is not concrete, operates lack of standardization, and technological parameter is imperfect, causes finished product utilization rate low.
Summary of the invention
It is an object of the invention to overcome the shortcoming of prior art, it is provided that a kind of zirconia ceramics material made for artificial tooth The manufacture method of material powder body.
The purpose of the present invention is achieved through the following technical solutions: a kind of zirconia ceramics material powder made for artificial tooth The manufacture method of body, it comprises the steps of:
S1. weigh: weigh each raw material by following weight ratio, standby:
Zirconium oxide: 6～17；Aluminium oxide: 0.5～1.0；Ceramics: 10～25；Starch: 25～48；Yittrium oxide: 3～12；Dispersion Agent: 0.5～2.5；Water-soluble binder: 1.5～3；
S2. making zirconia ceramics precursor, it comprises the following steps:
S21. grind: the zirconium oxide, aluminium oxide, ceramics, yittrium oxide and the dispersant that step S1 are weighed put in ball mill and grind Mill 1～3h, obtains milled mixtures；
S22. lyophilization: by the milled mixtures vacuum lyophilization 8～15h of step S21 gained；
S23. calcining: added in crucible by the milled mixtures after the gained lyophilization of step S22, adds starch and water-soluble Property binding agent, stirring obtain zirconia ceramics precursor；
S3. it is dried: carry out being vacuum dried 1～4h by the zirconia ceramics precursor of step S23 gained；
S4. ball milling: dried for step S3 gained zirconia ceramics precursor is placed in ball mill and carries out ball milling, aoxidized Zircon ceramic material powder.
Further, the preferred version that the ratio by weight of raw material described in step S1 weighs is: zirconium oxide: 12；Oxidation Aluminum: 0.8；Ceramics: 18；Starch: 36；Yittrium oxide: 8；Dispersant: 1.5；Water-soluble binder: 2.2.
Further, during described dispersant is dehydrated alcohol, polyacrylamide, triethyl group hexyl phosphoric acid or stearic acid Kind.
Further, described water-soluble binder is polyvinyl alcohol, xanthan gum, poly(ethylene oxide), methylcellulose or poly- One in vinylpyrrolidone.
Further, the condition of vacuum lyophilization described in step S22 is-35～-50 DEG C, and vacuum is 3～60Pa.
Further, described in step S23, the speed of stirring is 120～320rpm.
Further, vacuum drying condition described in step S3 is 200～400MPa.
Further, ball milling described in step S4 is wet ball grinding；The rotating speed of described ball mill is 400～700rpm；Institute The time stating ball milling is 2～3h.
Further, the particle diameter of described step S4 gained zirconia ceramics powder body is 20～40nm.
The invention have the advantages that the artificial tooth using the zirconia ceramics material powder body of the present invention to make has higher Hardness, adds dispersant in its composition, and therefore, the ceramic material of the present invention solves that All-ceramic material is frangible, glossiness is low, exhibition The problem that color is poor, transparency is low；The manufacture method of the zirconia ceramics material powder body that the present invention provides is simple to operate, specification, And the most perfect zirconia ceramics material powder body technological parameter in manufacturing process, improve finished product utilization rate, reduce Production cost.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, and protection scope of the present invention is not limited to following institute State.
Embodiment 1: the manufacture method of a kind of zirconia ceramics material powder body made for artificial tooth, it is by following steps group Become:
S1. weigh: weigh each raw material by following weight ratio, standby:
Zirconium oxide: 12；Aluminium oxide: 0.8；Ceramics: 18；Starch: 36；Yittrium oxide: 8；Dehydrated alcohol: 1.5；Polyvinyl alcohol: 2.2。
S2. making zirconia ceramics precursor, it comprises the following steps:
S21. grind: the zirconium oxide, aluminium oxide, ceramics, yittrium oxide and the dehydrated alcohol that step S1 are weighed put in ball mill Grind 1h, obtain milled mixtures；
S22. lyophilization: the milled mixtures of step S21 gained is-35 DEG C in temperature, vacuum be carry out under 3Pa cold The dry 8h of lyophilizing；
S23. calcining: the milled mixtures after the gained lyophilization of step S22 is added in crucible, adds starch and poly-second Enol, stirring obtains zirconia ceramics precursor；The speed of described stirring is 120rpm；
S3. it is dried: the zirconia ceramics precursor of step S23 gained is dried 1h under the vacuum condition of 200MPa；
S4. ball milling: dried for step S3 gained zirconia ceramics precursor is placed in ball mill and carries out wet ball grinding 2h, To zirconia ceramics material powder body；The rotating speed of described ball mill is 400rpm；The particle diameter of described zirconia ceramics powder body is 20nm.
Embodiment 2: the manufacture method of a kind of zirconia ceramics material powder body made for artificial tooth, it is by following steps group Become:
S1. weigh: weigh each raw material by following weight ratio, standby:
Zirconium oxide: 6；Aluminium oxide: 0.5；Ceramics: 10；Starch: 25；Yittrium oxide: 3；Polyacrylamide 0.5；Xanthan gum 1.5
S2. making zirconia ceramics precursor, it comprises the following steps:
S21. grind: the zirconium oxide, aluminium oxide, ceramics, yittrium oxide and the polyacrylamide that step S1 are weighed put into ball mill Middle grinding 3h, obtains milled mixtures；
S22. lyophilization: the milled mixtures of step S21 gained is-50 DEG C in temperature, under conditions of vacuum is 60Pa Carry out lyophilization 15h；
S23. calcining: the milled mixtures after the gained lyophilization of step S22 is added in crucible, adds starch and xanthan Glue, stirring obtains zirconia ceramics precursor；The speed of described stirring is 320rpm；
S3. it is dried: the zirconia ceramics precursor of step S23 gained is dried 4h under the vacuum condition of 400MPa；
S4. ball milling: dried for step S3 gained zirconia ceramics precursor is placed in ball mill and carries out wet ball grinding 3h, To zirconia ceramics material powder body；The rotating speed of described ball mill is 700rpm；The particle diameter of described zirconia ceramics powder body is 40nm.
Embodiment 3: the manufacture method of a kind of zirconia ceramics material powder body made for artificial tooth, it is by following steps group Become:
S1. weigh: weigh each raw material by following weight ratio, standby:
Zirconium oxide: 17；Aluminium oxide: 1.0；Ceramics: 25；Starch: 48；Yittrium oxide: 12；Triethyl group hexyl phosphoric acid: 2.5；Polycyclic Oxidative ethane: 3；
S2. making zirconia ceramics precursor, it comprises the following steps:
S21. grind: the zirconium oxide, aluminium oxide, ceramics, yittrium oxide and the triethyl group hexyl phosphoric acid that step S1 are weighed put into ball Grinding machine grinds 1.5h, obtains milled mixtures；
S22. lyophilization: the milled mixtures of step S21 gained is-45 DEG C in temperature, under conditions of vacuum is 35Pa Carry out lyophilization 13h；
S23. calcining: the milled mixtures after the gained lyophilization of step S22 is added in crucible, adds starch and polycyclic Oxidative ethane, stirring obtains zirconia ceramics precursor；The speed of described stirring is 215rpm；
S3. it is dried: the zirconia ceramics precursor of step S23 gained is dried 2.5h under the vacuum condition of 300MPa；
S4. ball milling: dried for step S3 gained zirconia ceramics precursor is placed in ball mill and carries out wet ball grinding 2.5h, Obtain zirconia ceramics material powder body；The rotating speed of described ball mill is 550rpm；The particle diameter of described zirconia ceramics powder body is 30nm。
Embodiment 4: the manufacture method of a kind of zirconia ceramics material powder body made for artificial tooth, it is by following steps group Become:
S1. weigh: weigh each raw material by following weight ratio, standby:
Zirconium oxide: 8；Aluminium oxide: 0.9；Ceramics: 22；Starch: 42；Yittrium oxide: 9；Stearic acid: 2.2；Methylcellulose: 2.8；
S2. making zirconia ceramics precursor, it comprises the following steps:
S21. grind: the zirconium oxide, aluminium oxide, ceramics, yittrium oxide and the stearic acid that step S1 are weighed put in ball mill and grind Mill 1.2h, obtains milled mixtures；
S22. lyophilization: the milled mixtures of step S21 gained is-39 DEG C in temperature, under conditions of vacuum is 10Pa Carry out lyophilization 10h；
S23. calcining: the milled mixtures after the gained lyophilization of step S22 is added in crucible, adds starch and methyl Cellulose, stirring obtains zirconia ceramics precursor；The speed of described stirring is 160rpm；
S3. it is dried: the zirconia ceramics precursor of step S23 gained is dried 1.5h under the vacuum condition of 220MPa；
S4. ball milling: dried for step S3 gained zirconia ceramics precursor is placed in ball mill and carries out wet ball grinding 2.2h, Obtain zirconia ceramics material powder body；The rotating speed of described ball mill is 450rpm；The particle diameter of described zirconia ceramics powder body is 25nm。
Embodiment 5: the manufacture method of a kind of zirconia ceramics material powder body made for artificial tooth, it is by following steps group Become:
S1. weigh: weigh each raw material by following weight ratio, standby:
Zirconium oxide: 15；Aluminium oxide: 0.6；Ceramics: 13；Starch: 29；Yittrium oxide: 4；Dehydrated alcohol: 0.9；Polyvinylpyrrolidine Ketone: 1.8；
S2. making zirconia ceramics precursor, it comprises the following steps:
S21. grind: the zirconium oxide, aluminium oxide, ceramics, yittrium oxide and the dehydrated alcohol that step S1 are weighed put in ball mill Grind 2.8h, obtain milled mixtures；
S22. lyophilization: the milled mixtures of step S21 gained is-46 DEG C in temperature, under conditions of vacuum is 55Pa Carry out lyophilization 13h；
S23. calcining: the milled mixtures after the gained lyophilization of step S22 is added in crucible, adds starch and poly-second Alkene pyrrolidone, stirring obtains zirconia ceramics precursor；The speed of described stirring is 280rpm；
S3. it is dried: the zirconia ceramics precursor of step S23 gained is dried 3.5h under the vacuum condition of 380MPa；
S4. ball milling: dried for step S3 gained zirconia ceramics precursor is placed in ball mill and carries out wet ball grinding 2.6h, Obtain zirconia ceramics material powder body；The rotating speed of described ball mill is 620rpm；The particle diameter of described zirconia ceramics powder body is 36nm。
Embodiment 6: the manufacture method of a kind of zirconia ceramics material powder body made for artificial tooth, it is by following steps group Become:
S1. weigh: weigh each raw material by following weight ratio, standby:
Zirconium oxide: 13；Aluminium oxide: 0.7；Ceramics: 20；Starch: 37；Yittrium oxide: 8；Polyacrylamide: 2；Polyvinyl alcohol: 2.4；
S2. making zirconia ceramics precursor, it comprises the following steps:
S21. grind: the zirconium oxide, aluminium oxide, ceramics, yittrium oxide and the polyacrylamide that step S1 are weighed put into ball mill Middle grinding 2h, obtains milled mixtures；
S22. lyophilization: the milled mixtures of step S21 gained is-45 DEG C in temperature, under conditions of vacuum is 20Pa Carry out lyophilization 10h；
S23. calcining: the milled mixtures after the gained lyophilization of step S22 is added in crucible, adds starch and poly-second Enol, stirring obtains zirconia ceramics precursor；The speed of described stirring is 240rpm；
S3. it is dried: the zirconia ceramics precursor of step S23 gained is dried under the vacuum condition of 200～400MPa 4h；
S4. ball milling: dried for step S3 gained zirconia ceramics precursor is placed in ball mill and carries out wet ball grinding 3h, To zirconia ceramics material powder body；The rotating speed of described ball mill is 600rpm；The particle diameter of described zirconia ceramics powder body is 32 nm。

Claims (9)

1. the manufacture method of the zirconia ceramics material powder body made for artificial tooth, it is characterised in that it is by following steps Composition:
S1. weigh: weigh each raw material by following weight ratio, standby:
Zirconium oxide: 6～17；Aluminium oxide: 0.5～1.0；Ceramics: 10～25；Starch: 25～48；Yittrium oxide: 3～12；Dispersion Agent: 0.5～2.5；Water-soluble binder: 1.5～3；
S2. making zirconia ceramics precursor, it comprises the following steps:
S21. grind: the zirconium oxide, aluminium oxide, ceramics, yittrium oxide and the dispersant that step S1 are weighed put in ball mill and grind Mill 1～3h, obtains milled mixtures；
S22. lyophilization: by the milled mixtures vacuum lyophilization 8～15h of step S21 gained；
S23. calcining: added in crucible by the milled mixtures after the gained lyophilization of step S22, adds starch and water-soluble Property binding agent, stirring obtain zirconia ceramics precursor；
S3. it is dried: carry out being vacuum dried 1～4h by the zirconia ceramics precursor of step S23 gained；
S4. ball milling: dried for step S3 gained zirconia ceramics precursor is placed in ball mill and carries out ball milling, aoxidized Zircon ceramic material powder.
A kind of manufacture method of the zirconia ceramics material powder body made for artificial tooth, its feature Being, the preferred version that the ratio by weight of raw material described in step S1 weighs is: zirconium oxide: 12；Aluminium oxide: 0.8；Pottery Powder: 18；Starch: 36；Yittrium oxide: 8；Dispersant: 1.5；Water-soluble binder: 2.2.
The manufacture method of a kind of zirconia ceramics material powder body made for artificial tooth, it is special Levying and be, described dispersant is the one in dehydrated alcohol, polyacrylamide, triethyl group hexyl phosphoric acid or stearic acid.
The manufacture method of a kind of zirconia ceramics material powder body made for artificial tooth, it is special Levying and be, described water-soluble binder is polyvinyl alcohol, xanthan gum, poly(ethylene oxide), methylcellulose or polyvinylpyrrolidine One in ketone.
A kind of manufacture method of the zirconia ceramics material powder body made for artificial tooth, step The condition of vacuum lyophilization described in S22 is-35～-50 DEG C, and vacuum is 3～60Pa.
A kind of manufacture method of the zirconia ceramics material powder body made for artificial tooth, step Described in S23, the speed of stirring is 120～320rpm.
A kind of manufacture method of the zirconia ceramics material powder body made for artificial tooth, step Vacuum drying condition described in S3 is 200～400MPa.
A kind of manufacture method of the zirconia ceramics material powder body made for artificial tooth, step Ball milling described in S4 is wet ball grinding；The rotating speed of described ball mill is 400～700rpm；The time of described ball milling is 2～3h.
A kind of manufacture method of the zirconia ceramics material powder body made for artificial tooth, described The particle diameter of step S4 gained zirconia ceramics powder body is 20～40nm.
CN201610275449.8A 2016-04-29 2016-04-29 Preparation method for zirconia ceramic material powder used for preparation of false tooth Pending CN105924157A (en)

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CN103641472A (en) * 2013-11-14 2014-03-19 厦门惠方生物科技有限公司 Method for preparing coloring semipermeable zirconia presintered body
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