CN110947029A - Manufacturing and weaving process of full-zirconia cellucotton and application thereof - Google Patents
Manufacturing and weaving process of full-zirconia cellucotton and application thereof Download PDFInfo
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/6225—Fibres based on zirconium oxide, e.g. zirconates such as PZT
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- 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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- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
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- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04C—BRAIDING OR MANUFACTURE OF LACE, INCLUDING BOBBIN-NET OR CARBONISED LACE; BRAIDING MACHINES; BRAID; LACE
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- D04C1/02—Braid or lace, e.g. pillow-lace; Processes for the manufacture thereof made from particular materials
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- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
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Abstract
The invention discloses a weaving process and application of full zirconia cellucotton, which comprises the following steps: (1) preparing powder; (2) preparing gel; (3) mixing; (4) filamentation; (5) weaving; (6) sintering; the fully zirconia fiber cotton prepared by the process is wound and woven into a screw base and a self-ligating bracket of the implant. The invention has the following advantages and effects: products with good ductility and toughness and high strength and compactness can be obtained; the composite material is applied to the screw base of the dental implant, has better biocompatibility, is more comfortable to use, and has better aesthetic appearance; is applied to the self-ligating bracket, and is more convenient to use.
Description
Technical Field
The invention relates to the technical field of oral medical treatment, in particular to a weaving process and application of full-zirconia cellucotton.
Background
Zirconia has the characteristics of inactive chemical property, high melting point, high resistivity, high refractive index and low thermal expansion coefficient, is an important high-temperature resistant material, a ceramic insulator material and a ceramic opacifier, is commonly used for manufacturing false teeth, namely zirconia full-porcelain teeth, has the characteristics of durability, vivid shape and being comparable to real teeth, and is popular among people. In addition, with the pursuit of beauty, the implantation of dental implants at the edentulous site is gradually started to fill the cavity of the edentulous. The implant structure that present oral cavity dental implantation operation adopted is mostly including the implant, the maintenance base station, wherein the similar expansion screw of implant structure, current implant is for guaranteeing intensity and life, adopt metal materials such as titanium alloy to make more, after the implant is planted and is accomplished, along with time slowly passes, it just begins to atrophy to plant the gum of planting tooth department, map out black expansion screw at corresponding gum department, thereby influence pleasing to the eye, in addition, because titanium alloy is relatively poor with human biocompatibility, the user can experience certain foreign matter and feel.
In addition, the existing chinese patent publication No. CN110078500A discloses a dental zirconia all-ceramic material and a preparation method thereof, wherein the dental zirconia all-ceramic material is prepared by the following preparation method: accurately weighing the raw materials for preparing the dental zirconia all-ceramic material according to a certain proportion: ceramic powder, pore-forming agent, binder, stabilizer and auxiliary agent; mixing ceramic powder, a stabilizing agent and at least part of auxiliary agent under the condition of a certain amount of solvent or no solvent, carrying out ball milling or sanding to obtain material powder, respectively adding a pore-forming agent, a binder and the rest of auxiliary agent into the material powder under the condition of heating or cooling to obtain material suspension, and placing the material suspension into a mould for cooling and drying to obtain the tooth zirconia all-ceramic material.
However, the zirconia all-ceramic material prepared by the preparation method has the following defects: the final material suspension is integrally formed in a mold, so that the ductility and toughness of the final material suspension are poor.
Disclosure of Invention
The invention aims to provide a manufacturing and weaving process of full-zirconia fiber cotton, and the prepared full-zirconia fiber cotton has better ductility and toughness. Another purpose is to provide the use of the all zirconia fiber cotton, when the screw base which is winded into the implant is woven by the all zirconia fiber cotton, the screw base has better aesthetic appearance and biocompatibility; when the self-ligating bracket is formed by winding the braid, the self-ligating bracket has a good automatic locking effect.
The technical purpose of the invention is realized by the following technical scheme:
a manufacturing and weaving process of full zirconia cellucotton comprises the following steps:
(1) preparing powder: taking zirconium oxide powder as a raw material, and grinding the zirconium oxide into particles with the diameter of 60-600 nm;
(2) preparing gel: mixing granular polyvinyl alcohol with water, and uniformly stirring to form homogeneous gel;
(3) mixing: adding the zirconium oxide particles prepared in the step (1) into the homogeneous gel prepared in the step (2) to obtain a homogeneous gel with zirconium oxide;
(4) filamentation: continuously pouring the homogeneous gel with the zirconia in the step (3) into a crucible with a leakage hole at the bottom, heating to 2700-3000 ℃ for continuous heating, volatilizing polyvinyl alcohol and water in the gel at the high temperature of 2700-3000 ℃, melting the zirconia in the gel at the high temperature of 2700-3000 ℃, continuously flowing the melted zirconia down from the leakage hole to form zirconia hot fluid, blowing cold air to the hot fluid in the horizontal direction by using cold air equipment, and quickly condensing the hot fluid by using the cold air to form filamentous full zirconia cellucotton;
(5) weaving: knitting the all-zirconia fiber cotton prepared in the step (4) in a knitting machine for forming;
(6) and (3) sintering: and (5) conveying the product formed by weaving in the step (5) into a pushed slab kiln for high-temperature sintering, and gradually cooling the pushed slab kiln at the rear part.
By adopting the technical scheme, the polyvinyl alcohol and the water in the step (2) are mixed according to a proper mass ratio to form gel, and the zirconium oxide small particles in the step (3) can be uniformly distributed in the gel, so that the zirconium oxide small particles can be conveniently heated and melted in a crucible in the subsequent step; since the melting point of the polyvinyl alcohol is 230-240 ℃, the polyvinyl alcohol generally starts to decompose when the temperature of the polyvinyl alcohol rises to more than 200 ℃ to generate water, acetic acid, acetaldehyde and crotonaldehyde, the boiling point of the water is 100 ℃, the boiling point of the acetic acid is 117.9 ℃, the boiling point of the acetaldehyde is 20.8 ℃, the boiling point of the crotonaldehyde is 102.2 ℃ and the melting point of the zirconium oxide is about 2700 ℃ and the boiling point of the zirconium oxide is 4300 ℃ under a standard atmospheric pressure, the temperature in the step (4) rises to 2700-3000 ℃ and the decomposition products are continuously heated, at the moment, the water, the polyvinyl alcohol and the decomposition products in the gel are volatilized, and only the zirconium oxide in a molten state is left. The product obtained after sintering in the step (6) has good ductility and toughness, and has high strength and compactness.
The invention is further provided with: and (5) setting the cold air equipment in the step (4) as an air cooler.
The invention is further provided with: in the step (2), the mass ratio of the polyvinyl alcohol to the water is 1: 9, and the stirring time is 1 hour or more.
By adopting the technical scheme, after the polyvinyl alcohol and the water are mixed according to the mass ratio of 1: 9, the formed gel is not too thin or too thick, and the gel uniformly mixed with the zirconia is suitable to be poured into a crucible.
The invention is further provided with: and (3) heating in the stirring process in the step (2), wherein the heating temperature is set to be 60-90 ℃.
By adopting the technical scheme, the heating is carried out in the stirring process, the heating can accelerate the dissolution of the polyvinyl alcohol and can also prevent agglomeration from influencing the dissolution speed.
The invention is further provided with: the heating temperature was set to 80 ℃.
By adopting the technical scheme, when the polyvinyl alcohol is dissolved in water to prepare the gel, the heating temperature is controlled to be 80 ℃, so that the gel is conveniently and naturally formed.
The invention is further provided with: the heating temperature in step (4) was set to 2700 ℃.
By adopting the technical scheme, the melting point of the zirconium oxide is 2680 ℃, so when the heating temperature is 2700 ℃, the zirconium oxide is in a molten state, and the temperature rise time of 2700 ℃ is shorter than that of 3000 ℃, so that energy can be saved to a certain extent.
The invention is further provided with: in the step (6), the sintering temperature is 1300-1800 ℃, and the sintering time is 8-12 h.
By adopting the technical scheme, the smaller the particles of the zirconia are, the lower the sintering temperature is in the step (6), the shorter the sintering time is, and the better the compactness and the higher strength are after sintering.
The invention is further provided with: in the step (6), the sintering temperature is 1600 ℃, and the sintering time is 11 h.
The other technical purpose of the invention is realized by the following technical scheme: the application of the fully zirconia fiber cotton is to weave the fully zirconia fiber cotton prepared in the step (4) into a screw base of the dental implant in a winding way.
By adopting the technical scheme, compared with the screw base made of titanium alloy in the prior art, the screw base made of the filamentous full-zirconia fiber cotton wound and woven has better biocompatibility, and a user feels less foreign body sensation and is more comfortable; in addition, the whole body of the artificial tooth is white, and the white screw base is closer to the color of the gum compared with the black screw base, so that the artificial tooth is more natural in appearance and has better aesthetic appearance.
The other technical purpose of the invention is realized by the following technical scheme: the utility model provides a usage of full zirconia cellucotton, twines the full zirconia cellucotton that makes in step (4) and weaves into self-ligating bracket, and self-ligating bracket is including holding in the palm the groove body, holds in the palm and is provided with pivot, fore shaft on the groove body, rotates in the pivot and connects the locking piece, and the one end that the pivot was kept away from to the locking piece is provided with the locking lug, and the locking lug locks the cooperation with the fore shaft locking.
Through adopting above-mentioned technical scheme, after filamentous full zirconia fiber cotton weaved into the self-ligating bracket, because have certain elasticity and the ductility of full zirconia fiber cotton self between silk and the silk for locking lug accessible elastic lock on the fore shaft, the arch wire that will pass the self-ligating bracket is locked, and it is more convenient to use.
In conclusion, the invention has the following beneficial effects:
1. mixing polyvinyl alcohol and water to prepare homogeneous gel by using zirconia small particles as raw materials, adding the zirconia small particles into the homogeneous gel with zirconia, uniformly stirring the homogeneous gel to form the homogeneous gel with the zirconia, pouring the homogeneous gel into a crucible with a leakage hole at the bottom, volatilizing the polyvinyl alcohol and the water at the high temperature of 2700 ℃ and 3000 ℃, melting the zirconia into liquid, continuously flowing the zirconia out of the leakage hole under the self gravity, blowing cold air by an air cooler, condensing to form filamentous full zirconia fiber cotton, and sintering after weaving, wherein the sintered product has good ductility, toughness, strength and compactness;
2. compared with a titanium alloy screw base, the screw base has better biocompatibility, and a user feels less foreign body sensation and is more comfortable; in addition, the whole body is white, and the white screw base is closer to the color of the gum compared with the black screw base, so that the appearance is more natural, and the appearance has better aesthetic appearance;
3. adopt filamentous full zirconia fiber cotton winding to weave into the self-ligating bracket, because have certain elasticity and the ductility of full zirconia fiber cotton self between silk and the silk for locking lug accessible elastic lock is on the fore shaft, will pass the arch wire locking in self-ligating bracket, and it is more convenient to use.
Drawings
FIG. 1 is a schematic view showing the overall structural relationship of a self-ligating bracket of example 2.
FIG. 2 is a schematic view showing the structure of the self-ligating bracket of embodiment 2 with the locking piece and the shaft separated from each other.
In the figure: 1. a bracket body; 2. a rotating shaft; 3. locking the opening; 4. a locking block; 41. a through hole; 42. the locking lug.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The materials, reagents and the like used in the examples are commercially available unless otherwise specified.
Example 1
A manufacturing and weaving process of full zirconia cellucotton and application thereof are disclosed, wherein the manufacturing process comprises the following steps:
(1) preparing powder: taking a proper amount of zirconia powder as a raw material, and grinding the zirconia into small particles with the diameter of 600nm +/-20 nm by adopting a ball milling mode.
(2) Preparing gel: mixing granular polyvinyl alcohol with water at a mass ratio of 1: 9, heating the mixture of polyvinyl alcohol and water to 80 ℃, and stirring for 1 hour to form homogeneous gel. Heating is carried out in the stirring process, the heating not only can accelerate the dissolution of the polyvinyl alcohol, but also can prevent agglomeration from influencing the dissolution speed, and when the polyvinyl alcohol is dissolved in water to prepare the gel, the heating temperature is controlled at 80 ℃, so that the gel is conveniently and naturally formed.
(3) Mixing: and (3) adding the zirconium oxide particles prepared in the step (1) into the homogeneous gel prepared in the step (2), and uniformly stirring to obtain the homogeneous gel with zirconium oxide, wherein the small zirconium oxide particles can be uniformly distributed in the homogeneous gel prepared in the step (2).
(4) Filamentation: and (3) continuously pouring the homogeneous gel with the zirconia prepared in the step (3) into a crucible with a leakage hole at the bottom, heating the crucible to 2700 ℃, and continuously heating, wherein the melting point of the polyvinyl alcohol is 230-240 ℃, the decomposition is started when the temperature of the polyvinyl alcohol is normally raised to be higher than 200 ℃, water, acetic acid, acetaldehyde and crotonaldehyde are generated, the boiling point of the water is 100 ℃, the boiling point of the acetic acid is 117.9 ℃, the boiling point of the acetaldehyde is 20.8 ℃, the boiling point of the crotonaldehyde is 102.2 ℃, the melting point of the zirconia is 2680 ℃, the boiling point of the zirconia is 4300 ℃, the water, the polyvinyl alcohol and decomposition products in the gel volatilize at 2700 ℃, and only the zirconia in a molten state is left. Zirconia flows down from tiny leak continuously by utilizing self gravity to form zirconia hot fluid, and simultaneously an air cooler is used for blowing cold air to the hot fluid in the horizontal direction, and the cold air enables the hot fluid to be rapidly condensed to form filamentous full zirconia cellucotton.
(5) Weaving: and (5) knitting the all-zirconia fiber cotton prepared in the step (4) into a screw base of the dental implant in a knitting machine.
(6) And (3) sintering: and (4) sending the screw base woven in the step (5) into a pushed slab kiln for high-temperature sintering at 1600 ℃ for 11h, and then gradually cooling at an outlet at the rear part of the pushed slab kiln. The smaller the particles of the zirconia are, the lower the sintering temperature is, the shorter the sintering time is, and the screw base obtained after sintering has better ductility and toughness and higher strength and compactness.
Compared with the screw base made of titanium alloy in the prior art, the screw base made of the filamentous full-zirconia fiber cotton in a winding and weaving mode has better biocompatibility, and a user feels less foreign body sensation and is more comfortable; in addition, the whole body of the artificial tooth is white, and the white screw base is closer to the color of the gum compared with the black screw base, so that the artificial tooth is more natural in appearance and has better aesthetic appearance.
Example 2
A manufacturing and weaving process of full zirconia cellucotton and application thereof are disclosed, wherein the manufacturing process comprises the following steps:
(1) preparing powder: taking a proper amount of zirconia powder as a raw material, and grinding the zirconia into small particles with the diameter of 200nm +/-10 nm by adopting a ball milling mode.
(2) Preparing gel: mixing granular polyvinyl alcohol with water at a mass ratio of 1: 9, heating the mixture of polyvinyl alcohol and water to 80 ℃, and stirring for 1 hour to form homogeneous gel. Heating is carried out in the stirring process, the heating not only can accelerate the dissolution of the polyvinyl alcohol, but also can prevent agglomeration from influencing the dissolution speed, and when the polyvinyl alcohol is dissolved in water to prepare the gel, the heating temperature is controlled at 80 ℃, so that the gel is conveniently and naturally formed.
(3) Mixing: and (3) adding the zirconium oxide particles prepared in the step (1) into the homogeneous gel prepared in the step (2), and uniformly stirring to obtain the homogeneous gel with zirconium oxide, wherein the small zirconium oxide particles can be uniformly distributed in the homogeneous gel prepared in the step (2).
(4) Filamentation: and (3) continuously pouring the homogeneous gel with the zirconia prepared in the step (3) into a crucible with a leak hole at the bottom, heating the crucible to 2900 ℃, and continuously heating, wherein the water, the polyvinyl alcohol and the decomposition products thereof in the gel volatilize at the temperature of 2900 ℃, and only the zirconia in a molten state is left. Zirconia flows down from tiny leak continuously by utilizing self gravity to form zirconia hot fluid, and simultaneously an air cooler is used for blowing cold air to the hot fluid in the horizontal direction, and the cold air enables the hot fluid to be rapidly condensed to form filamentous full zirconia cellucotton.
(5) Weaving: and (4) weaving the fully zirconia fiber cotton prepared in the step (4) into the self-ligating bracket in a weaving machine.
(6) And (3) sintering: and (3) sending the self-ligating bracket woven in the step (5) into a pushed slab kiln for high-temperature sintering at 1400 ℃ for 9h, and then naturally cooling at an outlet at the rear part of the pushed slab kiln.
As shown in fig. 1 and 2, the woven and sintered self-ligating bracket comprises a bracket body 1, a rotating shaft 2 and a locking notch 3 are arranged on the bracket body 1, a locking block 4 is rotatably connected to the rotating shaft 2, a through hole 41 is formed in the locking block 4, the rotating shaft 2 penetrates through the through hole 41, a locking lug 42 is arranged at one end, far away from the rotating shaft 2, of the locking block 4, and the locking lug 42 is in locking fit with the locking notch 3. After the filamentous full-zirconia fiber cotton is woven into the self-ligating bracket, the locking lug 42 can be locked on the locking notch 3 through elastic force, and an arch wire passing through the self-ligating bracket is locked, so that the use is more convenient.
The above description is only a preferred embodiment of the present invention, and all equivalent changes or modifications of the structure, characteristics and principles described in the present invention are included in the scope of the present invention.
Claims (10)
1. A manufacturing and weaving process of full zirconia cellucotton is characterized by comprising the following steps:
(1) preparing powder: taking zirconium oxide powder as a raw material, and grinding the zirconium oxide into particles with the diameter of 60-600 nm;
(2) preparing gel: mixing granular polyvinyl alcohol with water, and uniformly stirring to form homogeneous gel;
(3) mixing: adding the zirconium oxide particles prepared in the step (1) into the homogeneous gel prepared in the step (2) to obtain a homogeneous gel with zirconium oxide;
(4) filamentation: continuously pouring the homogeneous gel with the zirconia in the step (3) into a crucible with a leakage hole at the bottom, heating to 2700-3000 ℃ for continuous heating, volatilizing polyvinyl alcohol and water in the gel at the high temperature of 2700-3000 ℃, melting the zirconia in the gel at the high temperature of 2700-3000 ℃, continuously flowing the melted zirconia down from the leakage hole to form zirconia hot fluid, blowing cold air to the hot fluid in the horizontal direction by using cold air equipment, and quickly condensing the hot fluid by using the cold air to form filamentous full zirconia cellucotton;
(5) weaving: knitting the all-zirconia fiber cotton prepared in the step (4) in a knitting machine for forming;
(6) and (3) sintering: and (5) conveying the woven and formed product in the step (5) into a pushed slab kiln for high-temperature sintering, and gradually cooling the pushed slab kiln at the rear part.
2. The process for weaving fully zirconia fiber cotton according to claim 1, wherein the weaving process comprises the following steps: and (5) setting the cold air equipment in the step (4) as an air cooler.
3. The process for weaving fully zirconia fiber cotton according to claim 1, wherein the weaving process comprises the following steps: in the step (2), the mass ratio of the polyvinyl alcohol to the water is 1: 9, and the stirring time is 1 hour or more.
4. The process for weaving fully zirconia fiber cotton according to claim 1, wherein the weaving process comprises the following steps: and (3) heating in the stirring process in the step (2), wherein the heating temperature is set to be 60-90 ℃.
5. The process for weaving fully zirconia fiber cotton according to claim 4, wherein the weaving process comprises the following steps: the heating temperature was set at 80 ℃.
6. The process for weaving fully zirconia fiber cotton according to claim 1, wherein the weaving process comprises the following steps: the heating temperature in step (4) was set to 2700 ℃.
7. The process for weaving fully zirconia fiber cotton according to claim 1, wherein the weaving process comprises the following steps: in the step (6), the sintering temperature is 1300-1800 ℃, and the sintering time is 8-12 h.
8. The process for weaving fully zirconia fiber cotton according to claim 7, wherein the weaving process comprises the following steps: in the step (6), the sintering temperature is 1600 ℃, and the sintering time is 11 h.
9. The use of fully zirconia cellucotton, which is prepared by the process of claims 1 to 8, is characterized in that: and (4) winding and weaving the fully zirconia fiber cotton prepared in the step (4) into a screw base of the dental implant.
10. The use of fully zirconia cellucotton, which is prepared by the process of claims 1 to 8, is characterized in that: and (3) winding and weaving the full zirconia cellucotton prepared in the step (4) into a self-ligating bracket, wherein the self-ligating bracket comprises a bracket body, a rotating shaft and a locking notch are arranged on the bracket body, the rotating shaft is rotatably connected with a locking block, one end, far away from the rotating shaft, of the locking block is provided with a locking lug, and the locking lug is in locking fit with the locking notch.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911288596.9A CN110947029B (en) | 2019-12-16 | 2019-12-16 | Manufacturing and weaving process of full-zirconia cellucotton and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911288596.9A CN110947029B (en) | 2019-12-16 | 2019-12-16 | Manufacturing and weaving process of full-zirconia cellucotton and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110947029A true CN110947029A (en) | 2020-04-03 |
| CN110947029B CN110947029B (en) | 2022-03-01 |
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| CN112032751A (en) * | 2020-09-01 | 2020-12-04 | 成都龙之泉科技股份有限公司 | Chimney and steel matrix flue joint anticorrosive layer structure and preparation method thereof |
| CN112759389A (en) * | 2021-01-25 | 2021-05-07 | 上海大学绍兴研究院 | Zirconia fiber reinforced ceramic matrix composite artificial bone and preparation method thereof |
| CN112898037A (en) * | 2021-01-25 | 2021-06-04 | 上海大学绍兴研究院 | Full-zirconia ceramic dental implant and preparation method thereof |
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| CN112898037A (en) * | 2021-01-25 | 2021-06-04 | 上海大学绍兴研究院 | Full-zirconia ceramic dental implant and preparation method thereof |
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| CN110947029B (en) | 2022-03-01 |
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