CN117510204A - Composite ceramic traction buckle and preparation method thereof - Google Patents
Composite ceramic traction buckle and preparation method thereof Download PDFInfo
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- CN117510204A CN117510204A CN202311640303.5A CN202311640303A CN117510204A CN 117510204 A CN117510204 A CN 117510204A CN 202311640303 A CN202311640303 A CN 202311640303A CN 117510204 A CN117510204 A CN 117510204A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 168
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 145
- 239000008367 deionised water Substances 0.000 claims abstract description 136
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 136
- 239000000843 powder Substances 0.000 claims abstract description 130
- 239000002002 slurry Substances 0.000 claims abstract description 91
- 238000001035 drying Methods 0.000 claims abstract description 75
- 238000002156 mixing Methods 0.000 claims abstract description 71
- 238000000227 grinding Methods 0.000 claims abstract description 33
- 238000007873 sieving Methods 0.000 claims abstract description 28
- 238000010304 firing Methods 0.000 claims abstract description 27
- 238000001816 cooling Methods 0.000 claims abstract description 24
- 238000000748 compression moulding Methods 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims description 129
- 238000006243 chemical reaction Methods 0.000 claims description 86
- 238000003756 stirring Methods 0.000 claims description 77
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 60
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 54
- 239000011324 bead Substances 0.000 claims description 40
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 36
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 36
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 36
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 36
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 36
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 21
- 239000006185 dispersion Substances 0.000 claims description 21
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 claims description 20
- 239000008187 granular material Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 20
- 238000001238 wet grinding Methods 0.000 claims description 20
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 19
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 19
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 18
- JNQVLKWNKVMFBN-UHFFFAOYSA-N 2-hydroxy-n,n-dimethylacetamide Chemical compound CN(C)C(=O)CO JNQVLKWNKVMFBN-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 18
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 18
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 18
- 239000004359 castor oil Substances 0.000 claims description 18
- 235000019438 castor oil Nutrition 0.000 claims description 18
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 18
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 18
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 18
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 18
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 18
- 239000011780 sodium chloride Substances 0.000 claims description 18
- 239000007790 solid phase Substances 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 12
- 229920000058 polyacrylate Polymers 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 4
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000012937 correction Methods 0.000 abstract description 4
- 238000012216 screening Methods 0.000 description 23
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 10
- 230000008569 process Effects 0.000 description 6
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910002800 Si–O–Al Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000669 biting effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 235000021059 hard food Nutrition 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 210000002200 mouth mucosa Anatomy 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000013354 porous framework Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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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
- C04B35/622—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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
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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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
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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
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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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses a composite ceramic traction buckle and a preparation method thereof, belonging to the technical field of tooth correction. The preparation of the composite ceramic traction buckle comprises the following steps: mixing the first slurry with deionized water, ball milling, drying, grinding, granulating, drying, and sieving to obtain first powder; mixing and ball milling the second slurry, zirconia powder and deionized water, drying, grinding and granulating, drying and sieving to obtain second powder; uniformly paving the first powder in a die to obtain a first powder layer, uniformly paving the second powder on the first powder layer, and performing compression molding to obtain a ceramic green body; firing the ceramic green body at 1150-1250 ℃ and cooling to obtain a preform; and firing the preform at 1650-1700 ℃ and cooling to obtain the composite ceramic traction buckle, so that the fracture toughness of the ceramic traction buckle is improved, the possibility of breakage is reduced, and the durability is improved.
Description
Technical Field
The invention belongs to the technical field of tooth correction, and particularly relates to a composite ceramic traction buckle and a preparation method thereof.
Background
In the orthodontic treatment process, traction elements are required to apply traction force to the appliance to assist in orthodontic treatment, and ceramic traction buckles are common traction elements used in the orthodontic treatment process and used for connecting springs or rubber bands to teeth, and the positions and directions of the teeth are adjusted by applying proper force. Compared with the traditional metal traction buckle, the ceramic traction buckle is more attractive, and because the ceramic traction buckle adopts the ceramic material and has similar color with teeth, obvious visual influence can not be caused. In addition, the ceramic traction buckle has good biocompatibility, can be fully fused with oral tissues, and reduces the irritation and damage to oral mucosa. This makes ceramic traction buckles a common and desirable choice for achieving the desired effect in orthodontic treatment. However, ceramic materials have higher brittleness than metal materials because the bonding bonds between atoms of the ceramic materials are covalent bonds and ionic bonds, the covalent bonds have obvious directionality and saturation, and repulsive forces are large when ions of the same number as the ionic bonds are close, so ceramics mainly composed of ionic crystals and covalent crystals have little slip system, and generally break before slip occurs, so that the slip system of the ceramic materials is very small, and break phenomenon occurs when stress is applied. Therefore, when a patient bites hard food or bites abnormal objects, excessive force or violent biting action is applied to the teeth, so that the ceramic traction buckle breaks, the appliance loses traction function, the correction process is affected, and the ceramic traction buckle repair or replacement also consumes additional time and money, so that the orthodontic cost is increased.
Disclosure of Invention
The invention discloses a composite ceramic traction buckle and a preparation method thereof, belonging to the technical field of tooth correction. The preparation of the composite ceramic traction buckle comprises the following steps: mixing the first slurry with deionized water, ball milling, drying, grinding, granulating, drying, and sieving to obtain first powder; mixing and ball milling the second slurry, zirconia powder and deionized water, drying, grinding and granulating, drying and sieving to obtain second powder; uniformly paving the first powder in a die to obtain a first powder layer, uniformly paving the second powder on the first powder layer, and performing compression molding to obtain a ceramic green body; firing the ceramic green body at 1150-1250 ℃ and cooling to obtain a preform; and firing the preform at 1650-1700 ℃ and cooling to obtain the composite ceramic traction buckle.
The invention aims to solve the technical problems: preparing the composite ceramic traction buckle with good fracture toughness.
The aim of the invention can be achieved by the following technical scheme:
the preparation of the composite ceramic traction buckle comprises the following steps:
(1) Mixing the first slurry with deionized water, ball milling, drying, grinding, granulating, drying, and sieving to obtain first powder;
(2) Mixing and ball milling the second slurry, zirconia powder and deionized water, drying, grinding and granulating, drying and sieving to obtain second powder;
(3) Uniformly paving the first powder in a die to obtain a first powder layer, uniformly paving the second powder on the first powder layer, and performing compression molding to obtain a ceramic green body;
(4) Firing the ceramic green body at 1150-1250 ℃ for 2-3h, and cooling to 80-100 ℃ to obtain a preform;
(5) Firing the preform at 1650-1700 ℃ for 4-6h, and cooling to room temperature to obtain the composite ceramic traction buckle;
wherein:
the preparation of the first slurry in step (1) comprises the following steps;
mixing and stirring a dispersing agent and deionized water for 20-30min, adding zirconia powder, performing ultrasonic dispersion for 20-30min to obtain a dispersion liquid, adding ammonia water to adjust the pH of the dispersion liquid to 8-12, and stirring for 2-3h to obtain the first slurry;
the preparation of the second slurry in the step (2) comprises the following steps of
(21) Weighing montmorillonite, grinding, sieving, adding deionized water, stirring, standing, collecting upper suspension, centrifuging, and collecting solid phase to obtain material A;
(22) Mixing the material A, sodium chloride and deionized water, performing temperature control reaction, performing centrifugal separation, taking a solid phase, washing with water, and drying to obtain a material B;
(23) Mixing the material B with deionized water, stirring for 2-3h, adding octadecyl trimethyl ammonium chloride for temperature control reaction, filtering after the reaction is finished, washing, and drying to obtain a material C;
(24) Mixing the material C and isophorone diisocyanate in a reaction kettle, performing ultrasonic dispersion at 80 ℃ for 1-2 hours, adding polytetrahydrofuran ether glycol under the condition of introducing nitrogen, stirring, adding 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide and dibutyltin dilaurate, performing temperature control reaction, adding acetone, performing temperature control reaction continuously, adding triethylamine and deionized water after the reaction is finished, and stirring to obtain a material D;
(25) And mixing and stirring a sodium hydroxide solution and an aluminum trichloride hexahydrate solution to obtain a material E, adjusting the pH value of the material E to be 4.0-4.2, adding the material D, and stirring at room temperature for 20-30h to obtain the second slurry.
As a preferable technical scheme of the invention, in the step (1), the ball milling refers to wet milling for 4-6 hours by using zirconia beads, and the mass ratio of the first slurry to the deionized water to the zirconia beads is 1.5-2.5:1:1, a step of; the sieving refers to sieving by using a 80-100 mesh sieve;
In the step (2), the ball milling refers to wet milling for 6-8 hours by using zirconia beads, wherein the mass ratio of the second slurry to the zirconia powder to the deionized water to the zirconia beads is 1.2-1.8:0.5-0.6:1:1, a step of; the sieving refers to sieving with a 60-mesh sieve, sieving the granules passing through the sieve with an 80-mesh sieve, and taking the granules left on the 80-mesh sieve;
in the step (3), the pressing forming refers to the forming by applying pressure of 10-12MPa for maintaining the pressure for 1-2 min; the mass ratio of the first powder to the second powder is 75-80:45-65.
As a preferred technical scheme of the invention, in the preparation of the first slurry in the step (1), the mass ratio of the dispersant to the deionized water to the zirconia powder is 3.5-11.1:100:75-85.
As a preferable technical scheme of the invention, in the step (21), the proportioning ratio of the montmorillonite and the deionized water is 100-200g:3-4L; the stirring time is 6-8h, and the standing time is 12-14h.
As a preferable technical scheme of the invention, in the step (22), the mass ratio of the material A to the sodium chloride to the deionized water is 1-1.5:1-2:10-12; the temperature control reaction is carried out at 60-65 ℃ for 5-7h, and the temperature of drying is 100 ℃.
In the step (23), as a preferable technical scheme of the invention, the mass ratio of the material B to deionized water to octadecyl trimethyl ammonium chloride is 2-3:10-12:0.5-0.8; the temperature control reaction is carried out at 80 ℃ for 5-6 hours.
In the step (24), the mass ratio of the material C, isophorone diisocyanate, polytetrahydrofuran ether glycol, 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide, dibutyltin dilaurate, acetone, triethylamine and deionized water is 1-1.5:0.5-0.6:0.8-1:0.2-0.4:0.08-0.1:0.05-0.08:0.04-0.06:0.02-0.03:5-10:0.5-0.6:10; the first temperature control reaction is carried out for 2-3 hours under the oil bath condition of 80 ℃; the second temperature control reaction is carried out for 30-40min under the condition of 35 ℃ oil bath.
As a preferable technical scheme of the invention, in the step (25), the proportioning ratio of the sodium hydroxide solution, the aluminum trichloride hexahydrate and the material D is 10-20mL:0.26-0.27mg:1g.
In a preferred embodiment of the present invention, in the preparation of the first slurry in the step (1), the dispersant is any one of ammonium polyacrylate, ammonium citrate, sodium hexametaphosphate, and polyethylene glycol.
The composite ceramic traction buckle prepared by the preparation method is characterized by comprising a shell.
The invention has the beneficial effects that:
according to the composite ceramic traction buckle and the preparation method thereof disclosed by the invention, the modified montmorillonite loaded with the organic pore-forming agent is prepared, and a porous network skeleton structure is formed in the ceramic firing process, so that the overall strength of the prepared ceramic traction buckle is improved, breakage is not easy to occur, the capability of dispersing stress is improved, when a ceramic material is subjected to external impact or load, the porous skeleton can rapidly disperse energy, and the propagation speed of the impact or load is slowed down through strain conversion between interfaces, so that the toughness of the ceramic is effectively improved;
further, by preparing the aluminum column support montmorillonite structure and constructing a uniform microporous pore structure, the stress impact dispersing performance of the porous framework is further improved;
further, in the firing process, al and Zr are bonded with Si-O in montmorillonite to form Si-O-Al and Si-O-Zr, so that the expansion of cracks is restrained in the zirconia phase transition toughening process, the further expansion of the cracks is prevented, and the fracture toughness is improved;
further, by the secondary high-temperature sintering, zirconia crystals provided in the first slurry are secondarily crystallized, crystal grains grow again, internal micropores are wrapped inside the crystal grains and cannot be eliminated, the density of the ceramic traction buckle is moderately reduced, and therefore the toughness of the ceramic traction buckle is improved.
Detailed Description
In order to further describe the technical means and effects adopted by the present invention for achieving the intended purpose, the following detailed description is given below with reference to the embodiments, structures, features and effects according to the present invention.
Example 1
Preparation of the first slurry: mixing and stirring ammonium polyacrylate and deionized water for 20min, adding zirconia powder, performing ultrasonic dispersion for 20min to obtain a dispersion liquid, adding ammonia water with the concentration of 14.8mol/L to adjust the pH of the dispersion liquid to 8, and stirring for 2h to obtain a first slurry; the mass ratio of the ammonium polyacrylate, deionized water and zirconia powder is 3.5:100:75.
preparation of a second slurry:
(21) Weighing montmorillonite, grinding, sieving with 200 mesh sieve, adding deionized water, stirring for 6 hr, standing for 12 hr, collecting upper suspension, centrifuging, and collecting solid phase to obtain material A; the proportioning ratio of montmorillonite and deionized water is 100g:3L;
(22) Mixing the material A, sodium chloride and deionized water, performing temperature control reaction, performing centrifugal separation, taking a solid phase, washing with water, and drying to obtain a material B; the mass ratio of the material A to the sodium chloride to the deionized water is 1:1:10; the temperature control reaction is carried out for 5 hours at 60 ℃, and the temperature of drying is 100 ℃;
(23) Mixing the material B with deionized water, stirring for 2 hours, adding octadecyl trimethyl ammonium chloride for temperature control reaction, filtering after the reaction is finished, washing, and drying at 100 ℃ to obtain a material C; the mass ratio of the material B to deionized water to octadecyl trimethyl ammonium chloride is 2:10:0.5; the temperature control reaction is carried out at 80 ℃ for 5 hours;
(24) Mixing the material C and isophorone diisocyanate in a reaction kettle, performing ultrasonic dispersion at 80 ℃ for 1h, adding polytetrahydrofuran ether glycol under the condition of introducing nitrogen, stirring for 30min, adding 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide and dibutyltin dilaurate, performing constant temperature reaction at 80 ℃ for 2h, adding acetone, performing constant temperature reaction at 35 ℃ for 30min, adding triethylamine and deionized water after the reaction is finished, and stirring for 2-3h to obtain a material D; the mass ratio of the materials C, isophorone diisocyanate, polytetrahydrofuran ether glycol, 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide, dibutyltin dilaurate, acetone, triethylamine and deionized water is 1:0.5:0.8:0.2:0.08:0.05:0.04:0.02:5:0.5:10;
(25) Mixing and stirring 0.2mol/L sodium hydroxide solution and 0.2mol/L aluminum chloride hexahydrate solution to obtain a material E, adjusting the pH value of the material E to 4.0, adding the material D, and stirring at room temperature for 20 hours to obtain a second slurry; the proportioning ratio of the sodium hydroxide solution, the aluminum chloride hexahydrate and the material D is 10mL:0.26mg:1g.
Preparation of a composite ceramic traction buckle:
(1) Mixing the first slurry and deionized water, wet-grinding for 4 hours by using zirconia beads, drying for 4 hours at 100 ℃, grinding, granulating, drying, and screening by using a 80-mesh screen to obtain first powder; the mass ratio of the first slurry to the deionized water to the zirconia beads is 1.5:1:1, a step of;
(2) Mixing the second slurry, zirconia powder and deionized water, wet-grinding for 6 hours by using zirconia beads, drying at 100 ℃ for 5 hours, grinding, granulating, drying, screening by a 60-mesh screen, screening the granules passing through the screen by a 80-mesh screen, and taking the granules left on the 80-mesh screen to obtain second powder; the mass ratio of the second slurry to the zirconia powder to the deionized water to the zirconia beads is 1.2:0.5:1:1, a step of;
(3) Uniformly paving the first powder in a die to obtain a first powder layer, uniformly paving the second powder on the first powder layer, and applying 10MPa pressure to maintain the pressure for 1min for compression molding to obtain a ceramic green body; the mass ratio of the first powder to the second powder is 75:45;
(4) Firing the ceramic green body at 1150 ℃ for 2 hours, and cooling to 80 ℃ to obtain a preform;
(5) And firing the preform at 1650 ℃ for 4 hours, and cooling to room temperature to obtain the composite ceramic traction buckle.
Example 2
Preparation of the first slurry: mixing and stirring ammonium citrate and deionized water for 22min, adding zirconia powder, performing ultrasonic dispersion for 22min to obtain a dispersion liquid, adding ammonia water with the concentration of 14.8mol/L to adjust the pH of the dispersion liquid to 9, and stirring for 2.2h to obtain first slurry; the mass ratio of the ammonium citrate to the deionized water to the zirconia powder is 5.5:100:78.
preparation of a second slurry:
(21) Weighing montmorillonite, grinding, sieving with 200 mesh sieve, adding deionized water, stirring for 6.5 hr, standing for 12.5 hr, collecting upper suspension, centrifuging, and collecting solid phase to obtain material A; the proportioning ratio of montmorillonite and deionized water is 130g:3.2L;
(22) Mixing the material A, sodium chloride and deionized water, performing temperature control reaction, performing centrifugal separation, taking a solid phase, washing with water, and drying to obtain a material B; the mass ratio of the material A to the sodium chloride to the deionized water is 1.2:1.2:10.5; the temperature control reaction is carried out for 6 hours at 62 ℃, and the temperature of drying is 100 ℃;
(23) Mixing the material B with deionized water, stirring for 2.5h, adding octadecyl trimethyl ammonium chloride for temperature control reaction, filtering after the reaction is finished, washing, and drying at 100 ℃ to obtain a material C; the mass ratio of the material B to deionized water to octadecyl trimethyl ammonium chloride is 2.5:10.5:0.6; the temperature control reaction is carried out at 80 ℃ for 5.5 hours;
(24) Mixing the material C and isophorone diisocyanate in a reaction kettle, performing ultrasonic dispersion at 80 ℃ for 1.5 hours, adding polytetrahydrofuran ether glycol under the condition of introducing nitrogen, stirring for 35 minutes, adding 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide and dibutyltin dilaurate, performing constant temperature reaction at 80 ℃ for 2.5 hours, adding acetone, performing constant temperature reaction at 35 ℃ for 35 minutes, adding triethylamine and deionized water after the reaction is finished, and stirring for 2.5 hours to obtain a material D; the mass ratio of the materials C, isophorone diisocyanate, polytetrahydrofuran ether glycol, 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide, dibutyltin dilaurate, acetone, triethylamine and deionized water is 1.2:0.55:0.88:0.25:0.088:0.058:0.045:0.025:6:0.55:10;
(25) Mixing and stirring 0.2mol/L sodium hydroxide solution and 0.2mol/L aluminum chloride hexahydrate solution to obtain a material E, adjusting the pH of the material E to 4.1, adding the material D, and stirring at room temperature for 25 hours to obtain a second slurry; the proportioning ratio of the sodium hydroxide solution, the aluminum chloride hexahydrate and the material D is 15mL:0.265mg:1g.
Preparation of a composite ceramic traction buckle:
(1) Mixing the first slurry and deionized water, wet-grinding for 5 hours by using zirconia beads, drying for 4 hours at 100 ℃, grinding, granulating, drying, and screening by using a 90-mesh screen to obtain first powder; the mass ratio of the first slurry to the deionized water to the zirconia beads is 2:1:1, a step of;
(2) Mixing the second slurry, zirconia powder and deionized water, wet-grinding for 7h by using zirconia beads, drying at 100 ℃ for 5h, grinding, granulating, drying, screening by a 60-mesh screen, screening the granules passing through the screen by a 80-mesh screen, and taking the granules left on the 80-mesh screen to obtain second powder; the mass ratio of the second slurry to the zirconia powder to the deionized water to the zirconia beads is 1.5:0.55:1:1, a step of;
(3) Uniformly paving the first powder in a die to obtain a first powder layer, uniformly paving the second powder on the first powder layer, and applying pressure of 11MPa for maintaining pressure for 1.5min for compression molding to obtain a ceramic green body; the mass ratio of the first powder to the second powder is 78:50;
(4) Firing the ceramic green body at 1180 ℃ for 2.5 hours, and cooling to 85 ℃ to obtain a preform;
(5) And firing the preform at 1680 ℃ for 4.5 hours, and cooling to room temperature to obtain the composite ceramic traction buckle.
Example 3
Preparation of the first slurry: mixing and stirring sodium hexametaphosphate and deionized water for 28min, adding zirconia powder, performing ultrasonic dispersion for 28min to obtain a dispersion liquid, adding ammonia water with the concentration of 14.8mol/L to adjust the pH of the dispersion liquid to 11, and stirring for 2.8h to obtain first slurry; the mass ratio of the sodium hexametaphosphate to the deionized water to the zirconia powder is 8.7:100:82.
preparation of a second slurry:
(21) Weighing montmorillonite, grinding, sieving with 200 mesh sieve, adding deionized water, stirring for 7h, standing for 13h, collecting upper suspension, centrifuging, and collecting solid phase to obtain material A; the proportioning ratio of montmorillonite and deionized water is 180g:3.7L;
(22) Mixing the material A, sodium chloride and deionized water, performing temperature control reaction, performing centrifugal separation, taking a solid phase, washing with water, and drying to obtain a material B; the mass ratio of the material A to the sodium chloride to the deionized water is 1.3:1.8:11.2; the temperature control reaction is carried out for 6.5 hours at 63 ℃, and the temperature of drying is 100 ℃;
(23) Mixing the material B with deionized water, stirring for 2.8h, adding octadecyl trimethyl ammonium chloride for temperature control reaction, filtering after the reaction is finished, washing, and drying at 100 ℃ to obtain a material C; the mass ratio of the material B to deionized water to octadecyl trimethyl ammonium chloride is 2.8:11.6:0.68; the temperature control reaction is carried out at 80 ℃ for 5.8 hours;
(24) Mixing the material C and isophorone diisocyanate in a reaction kettle, performing ultrasonic dispersion at 80 ℃ for 1.8 hours, adding polytetrahydrofuran ether glycol under the condition of introducing nitrogen, stirring for 38 minutes, adding 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide and dibutyltin dilaurate, performing constant temperature reaction at 80 ℃ for 2.8 hours, adding acetone, performing constant temperature reaction at 35 ℃ for 38 minutes, adding triethylamine and deionized water after the reaction is finished, and stirring for 2.8 hours to obtain a material D; the mass ratio of the materials C, isophorone diisocyanate, polytetrahydrofuran ether glycol, 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide, dibutyltin dilaurate, acetone, triethylamine and deionized water is 1.4:0.59:0.95:0.35:0.095:0.075:0.055:0.028:9:0.58:10;
(25) Mixing and stirring 0.2mol/L sodium hydroxide solution and 0.2mol/L aluminum chloride hexahydrate solution to obtain a material E, adjusting the pH of the material E to 4.1, adding the material D, and stirring at room temperature for 28 hours to obtain a second slurry; the proportioning ratio of the sodium hydroxide solution, the aluminum chloride hexahydrate and the material D is 18mL:0.268mg:1g.
Preparation of a composite ceramic traction buckle:
(1) Mixing the first slurry and deionized water, wet-milling by using zirconia beads for 5.8 hours, drying at 100 ℃ for 4 hours, grinding, granulating, drying, and sieving by using a 80-mesh sieve to obtain first powder; the mass ratio of the first slurry to the deionized water to the zirconia beads is 2.2:1:1, a step of;
(2) Mixing the second slurry, zirconia powder and deionized water, wet-grinding for 7.8 hours by using zirconia beads, drying at 100 ℃ for 5 hours, grinding, granulating, drying, screening by using a 60-mesh screen, screening the granules passing through the screen by using an 80-mesh screen, and taking the granules left on the 80-mesh screen to obtain second powder; the mass ratio of the second slurry to the zirconia powder to the deionized water to the zirconia beads is 1.6:0.58:1:1, a step of;
(3) Uniformly paving the first powder in a die to obtain a first powder layer, uniformly paving the second powder on the first powder layer, and applying pressure of 11.5MPa for 1.8min for compression molding to obtain a ceramic green body; the mass ratio of the first powder to the second powder is 79:62;
(4) Firing the ceramic green body at 1225 ℃ for 2.8 hours, and cooling to 95 ℃ to obtain a preform;
(5) And firing the preform at 1690 ℃ for 5.5 hours, and cooling to room temperature to obtain the composite ceramic traction buckle.
Example 4
Preparation of the first slurry: mixing polyethylene glycol and deionized water, stirring for 30min, adding zirconia powder, performing ultrasonic dispersion for 30min to obtain a dispersion liquid, adding ammonia water with the concentration of 14.8mol/L to adjust the pH of the dispersion liquid to 12, and stirring for 3h to obtain a first slurry; the mass ratio of the polyethylene glycol to the deionized water to the zirconia powder is 11.1:100:85.
preparation of a second slurry:
(21) Weighing montmorillonite, grinding, sieving with 200 mesh sieve, adding deionized water, stirring for 8 hr, standing for 14 hr, collecting upper suspension, centrifuging, and collecting solid phase to obtain material A; the proportioning ratio of montmorillonite and deionized water is 200g:4L;
(22) Mixing the material A, sodium chloride and deionized water, performing temperature control reaction, performing centrifugal separation, taking a solid phase, washing with water, and drying to obtain a material B; the mass ratio of the material A to the sodium chloride to the deionized water is 1.5:2:12; the temperature control reaction is carried out for 7 hours at 65 ℃, and the temperature of drying is 100 ℃;
(23) Mixing the material B with deionized water, stirring for 3 hours, adding octadecyl trimethyl ammonium chloride for temperature control reaction, filtering after the reaction is finished, washing, and drying at 100 ℃ to obtain a material C; the mass ratio of the material B to deionized water to octadecyl trimethyl ammonium chloride is 3:12:0.8; the temperature control reaction is to react for 6 hours at 80 ℃;
(24) Mixing the material C and isophorone diisocyanate in a reaction kettle, performing ultrasonic dispersion at 80 ℃ for 2 hours, adding polytetrahydrofuran ether glycol under the condition of introducing nitrogen, stirring for 40 minutes, adding 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide and dibutyltin dilaurate, performing constant temperature reaction at 80 ℃ for 3 hours, adding acetone, performing constant temperature reaction at 35 ℃ for 40 minutes, adding triethylamine and deionized water after the reaction is finished, and stirring for 3 hours to obtain a material D; the mass ratio of the materials C, isophorone diisocyanate, polytetrahydrofuran ether glycol, 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide, dibutyltin dilaurate, acetone, triethylamine and deionized water is 1.5:0.6:1:0.4:0.1:0.08:0.06:0.03:10:0.6:10;
(25) Mixing and stirring 0.2mol/L sodium hydroxide solution and 0.2mol/L aluminum chloride hexahydrate solution to obtain a material E, adjusting the pH value of the material E to 4.2, adding the material D, and stirring at room temperature for 30 hours to obtain a second slurry; the proportioning ratio of the sodium hydroxide solution, the aluminum chloride hexahydrate and the material D is 20mL:0.27mg:1g.
Preparation of a composite ceramic traction buckle:
(1) Mixing the first slurry and deionized water, wet-grinding for 6 hours by using zirconia beads, drying for 4 hours at 100 ℃, grinding, granulating, drying, and screening by using a 100-mesh screen to obtain first powder; the mass ratio of the first slurry to the deionized water to the zirconia beads is 2.5:1:1, a step of;
(2) Mixing the second slurry, zirconia powder and deionized water, wet-milling for 8 hours by using zirconia beads, drying at 100 ℃ for 5 hours, grinding, granulating, drying, screening by using a 60-mesh screen, screening the granules passing through the screen by using an 80-mesh screen, and taking the granules left on the 80-mesh screen to obtain second powder; the mass ratio of the second slurry to the zirconia powder to the deionized water to the zirconia beads is 1.8:0.6:1:1, a step of;
(3) Uniformly paving the first powder in a die to obtain a first powder layer, uniformly paving the second powder on the first powder layer, and applying 12MPa of pressure to maintain the pressure for 2min for compression molding to obtain a ceramic green body; the mass ratio of the first powder to the second powder is 80: 65.
(4) Firing the ceramic green body at 1250 ℃ for 3 hours, and cooling to 100 ℃ to obtain a preform;
(5) And firing the preform for 6 hours at 1700 ℃, and cooling to room temperature to obtain the composite ceramic traction buckle.
Comparative example 1
Preparation of the first slurry: mixing and stirring ammonium polyacrylate and deionized water for 20min, adding zirconia powder, performing ultrasonic dispersion for 20min to obtain a dispersion liquid, adding ammonia water with the concentration of 14.8mol/L to adjust the pH of the dispersion liquid to 8, and stirring for 2h to obtain a first slurry; the mass ratio of the ammonium polyacrylate, deionized water and zirconia powder is 3.5:100:75.
preparation of a ceramic traction buckle:
(1) Mixing the first slurry and deionized water, wet-grinding for 4 hours by using zirconia beads, drying for 4 hours at 100 ℃, grinding, granulating, drying, and screening by using a 80-mesh screen to obtain first powder; the mass ratio of the first slurry to the deionized water to the zirconia beads is 1.5:1:1, a step of;
(2) Uniformly spreading 120 parts by mass of the first powder in a die, and applying 10MPa pressure to maintain the pressure for 1min for compression molding to obtain a ceramic green body;
(3) Firing the ceramic green body at 1150 ℃ for 2 hours, and cooling to 80 ℃ to obtain a preform;
(4) And firing the preform at 1650 ℃ for 4 hours, and cooling to room temperature to obtain the ceramic traction buckle.
Comparative example 2
Preparation of a second slurry:
(21) Weighing montmorillonite, grinding, sieving with 200 mesh sieve, adding deionized water, stirring for 6 hr, standing for 12 hr, collecting upper suspension, centrifuging, and collecting solid phase to obtain material A; the proportioning ratio of montmorillonite and deionized water is 100g:3L;
(22) Mixing the material A, sodium chloride and deionized water, performing temperature control reaction, performing centrifugal separation, taking a solid phase, washing with water, and drying to obtain a material B; the mass ratio of the material A to the sodium chloride to the deionized water is 1:1:10; the temperature control reaction is carried out for 5 hours at 60 ℃, and the temperature of drying is 100 ℃;
(23) Mixing the material B with deionized water, stirring for 2 hours, adding octadecyl trimethyl ammonium chloride for temperature control reaction, filtering after the reaction is finished, washing, and drying at 100 ℃ to obtain a material C; the mass ratio of the material B to deionized water to octadecyl trimethyl ammonium chloride is 2:10:0.5; the temperature control reaction is carried out at 80 ℃ for 5 hours;
(24) Mixing the material C and isophorone diisocyanate in a reaction kettle, performing ultrasonic dispersion at 80 ℃ for 1h, adding polytetrahydrofuran ether glycol under the condition of introducing nitrogen, stirring for 30min, adding 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide and dibutyltin dilaurate, performing constant temperature reaction at 80 ℃ for 2h, adding acetone, performing constant temperature reaction at 35 ℃ for 30min, adding triethylamine and deionized water after the reaction is finished, and stirring for 2-3h to obtain a material D; the mass ratio of the materials C, isophorone diisocyanate, polytetrahydrofuran ether glycol, 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide, dibutyltin dilaurate, acetone, triethylamine and deionized water is 1:0.5:0.8:0.2:0.08:0.05:0.04:0.02:5:0.5:10;
(25) Mixing and stirring 0.2mol/L sodium hydroxide solution and 0.2mol/L aluminum chloride hexahydrate solution to obtain a material E, adjusting the pH value of the material E to 4.0, adding the material D, and stirring at room temperature for 20 hours to obtain a second slurry; the proportioning ratio of the sodium hydroxide solution, the aluminum chloride hexahydrate and the material D is 10mL:0.26mg:1g.
Preparation of a composite ceramic traction buckle:
(1) Mixing the second slurry, zirconia powder and deionized water, wet-grinding for 6 hours by using zirconia beads, drying at 100 ℃ for 5 hours, grinding, granulating, drying, screening by a 60-mesh screen, screening the granules passing through the screen by a 80-mesh screen, and taking the granules left on the 80-mesh screen to obtain second powder; the mass ratio of the second slurry to the zirconia powder to the deionized water to the zirconia beads is 1.2:0.5:1:1, a step of;
(2) Uniformly spreading 120 parts by mass of the second powder in a die, and applying 10MPa pressure to maintain the pressure for 1min for compression molding to obtain a ceramic green body;
(3) Firing the ceramic green body at 1150 ℃ for 2 hours, and cooling to 80 ℃ to obtain a preform;
(4) And firing the preform at 1650 ℃ for 4 hours, and cooling to room temperature to obtain the composite ceramic traction buckle.
Comparative example 3
Preparation of the first slurry: mixing and stirring ammonium polyacrylate and deionized water for 20min, adding zirconia powder, performing ultrasonic dispersion for 20min to obtain a dispersion liquid, adding ammonia water with the concentration of 14.8mol/L to adjust the pH of the dispersion liquid to 8, and stirring for 2h to obtain a first slurry; the mass ratio of the ammonium polyacrylate, deionized water and zirconia powder is 3.5:100:75.
Preparation of a second slurry:
mixing and stirring 0.2mol/L sodium hydroxide solution and 0.2mol/L aluminum chloride hexahydrate solution to obtain a material E, and adjusting the pH value of the material E to 4.0 to obtain second slurry; the proportioning ratio of the sodium hydroxide solution to the aluminum chloride hexahydrate is 10mL:0.26mg.
Preparation of a composite ceramic traction buckle:
(1) Mixing the first slurry and deionized water, wet-grinding for 4 hours by using zirconia beads, drying for 4 hours at 100 ℃, grinding, granulating, drying, and screening by using a 80-mesh screen to obtain first powder; the mass ratio of the first slurry to the deionized water to the zirconia beads is 1.5:1:1, a step of;
(2) Mixing the second slurry, zirconia powder and deionized water, wet-grinding for 6 hours by using zirconia beads, drying at 100 ℃ for 5 hours, grinding, granulating, drying, screening by a 60-mesh screen, screening the granules passing through the screen by a 80-mesh screen, and taking the granules left on the 80-mesh screen to obtain second powder; the mass ratio of the second slurry to the zirconia powder to the deionized water to the zirconia beads is 1.2:0.5:1:1, a step of;
(3) Uniformly paving the first powder in a die to obtain a first powder layer, uniformly paving the second powder on the first powder layer, and applying 10MPa pressure to maintain the pressure for 1min for compression molding to obtain a ceramic green body; the mass ratio of the first powder to the second powder is 75:45;
(4) Firing the ceramic green body at 1150 ℃ for 2 hours, and cooling to 80 ℃ to obtain a preform;
(5) And firing the preform at 1650 ℃ for 4 hours, and cooling to room temperature to obtain the composite ceramic traction buckle.
Comparative example 4
Preparation of the first slurry: mixing and stirring ammonium polyacrylate and deionized water for 20min, adding zirconia powder, performing ultrasonic dispersion for 20min to obtain a dispersion liquid, adding ammonia water with the concentration of 14.8mol/L to adjust the pH of the dispersion liquid to 8, and stirring for 2h to obtain a first slurry; the mass ratio of the ammonium polyacrylate, deionized water and zirconia powder is 3.5:100:75.
preparation of a second slurry:
(21) Weighing montmorillonite, grinding, sieving with 200 mesh sieve, adding deionized water, stirring for 6 hr, standing for 12 hr, collecting upper suspension, centrifuging, and collecting solid phase to obtain material A; the proportioning ratio of montmorillonite and deionized water is 100g:3L;
(22) Mixing the material A, sodium chloride and deionized water, performing temperature control reaction, performing centrifugal separation, taking a solid phase, washing with water, and drying to obtain a material B; the mass ratio of the material A to the sodium chloride to the deionized water is 1:1:10; the temperature control reaction is carried out for 5 hours at 60 ℃, and the temperature of drying is 100 ℃;
(23) Mixing the material B with deionized water, stirring for 2 hours, adding octadecyl trimethyl ammonium chloride for temperature control reaction, filtering after the reaction is finished, washing, and drying at 100 ℃ to obtain a material C; the mass ratio of the material B to deionized water to octadecyl trimethyl ammonium chloride is 2:10:0.5; the temperature control reaction is carried out at 80 ℃ for 5 hours;
(24) Mixing the material C and isophorone diisocyanate in a reaction kettle, performing ultrasonic dispersion at 80 ℃ for 1h, adding polytetrahydrofuran ether glycol under the condition of introducing nitrogen, stirring for 30min, adding 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide and dibutyltin dilaurate, performing constant temperature reaction at 80 ℃ for 2h, adding acetone, performing constant temperature reaction at 35 ℃ for 30min, adding triethylamine and deionized water after the reaction is finished, and stirring for 2-3h to obtain a material D; the mass ratio of the materials C, isophorone diisocyanate, polytetrahydrofuran ether glycol, 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide, dibutyltin dilaurate, acetone, triethylamine and deionized water is 1:0.5:0.8:0.2:0.08:0.05:0.04:0.02:5:0.5:10;
(25) Mixing and stirring 0.2mol/L sodium hydroxide solution and 0.2mol/L aluminum chloride hexahydrate solution to obtain a material E, adjusting the pH value of the material E to 4.0, adding the material D, and stirring at room temperature for 20 hours to obtain a second slurry; the proportioning ratio of the sodium hydroxide solution, the aluminum chloride hexahydrate and the material D is 10mL:0.26mg:1g.
Preparation of a composite ceramic traction buckle:
(1) Mixing the first slurry and deionized water, wet-grinding for 4 hours by using zirconia beads, drying for 4 hours at 100 ℃, grinding, granulating, drying, and screening by using a 80-mesh screen to obtain first powder; the mass ratio of the first slurry to the deionized water to the zirconia beads is 1.5:1:1, a step of;
(2) Mixing the second slurry, zirconia powder and deionized water, wet-grinding for 6 hours by using zirconia beads, drying at 100 ℃ for 5 hours, grinding, granulating, drying, screening by a 60-mesh screen, screening the granules passing through the screen by a 80-mesh screen, and taking the granules left on the 80-mesh screen to obtain second powder; the mass ratio of the second slurry to the zirconia powder to the deionized water to the zirconia beads is 1.2:0.5:1:1, a step of;
(3) Uniformly paving the first powder in a die to obtain a first powder layer, uniformly paving the second powder on the first powder layer, and applying 10MPa pressure to maintain the pressure for 1min for compression molding to obtain a ceramic green body; the mass ratio of the first powder to the second powder is 75:45;
(4) And firing the ceramic green body at 1150 ℃ for 6 hours, and cooling to room temperature to obtain the composite ceramic traction buckle.
Comparative example 5
Preparation of the first slurry: mixing and stirring ammonium polyacrylate and deionized water for 20min, adding zirconia powder, performing ultrasonic dispersion for 20min to obtain a dispersion liquid, adding ammonia water with the concentration of 14.8mol/L to adjust the pH of the dispersion liquid to 8, and stirring for 2h to obtain a first slurry; the mass ratio of the ammonium polyacrylate, deionized water and zirconia powder is 3.5:100:75.
preparation of a second slurry:
(21) Weighing montmorillonite, grinding, sieving with 200 mesh sieve, adding deionized water, stirring for 6 hr, standing for 12 hr, collecting upper suspension, centrifuging, and collecting solid phase to obtain material A; the proportioning ratio of montmorillonite and deionized water is 100g:3L;
(22) Mixing the material A, sodium chloride and deionized water, performing temperature control reaction, performing centrifugal separation, taking a solid phase, washing with water, and drying to obtain a material B; the mass ratio of the material A to the sodium chloride to the deionized water is 1:1:10; the temperature control reaction is carried out for 5 hours at 60 ℃, and the temperature of drying is 100 ℃;
(23) Mixing the material B with deionized water, stirring for 2 hours, adding octadecyl trimethyl ammonium chloride for temperature control reaction, filtering after the reaction is finished, washing, and drying at 100 ℃ to obtain a material C; the mass ratio of the material B to deionized water to octadecyl trimethyl ammonium chloride is 2:10:0.5; the temperature control reaction is carried out at 80 ℃ for 5 hours;
(24) Mixing the material C and isophorone diisocyanate in a reaction kettle, performing ultrasonic dispersion at 80 ℃ for 1h, adding polytetrahydrofuran ether glycol under the condition of introducing nitrogen, stirring for 30min, adding 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide and dibutyltin dilaurate, performing constant temperature reaction at 80 ℃ for 2h, adding acetone, performing constant temperature reaction at 35 ℃ for 30min, adding triethylamine and deionized water after the reaction is finished, and stirring for 2-3h to obtain a material D; the mass ratio of the materials C, isophorone diisocyanate, polytetrahydrofuran ether glycol, 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide, dibutyltin dilaurate, acetone, triethylamine and deionized water is 1:0.5:0.8:0.2:0.08:0.05:0.04:0.02:5:0.5:10;
(25) Mixing and stirring 0.2mol/L sodium hydroxide solution and 0.2mol/L aluminum chloride hexahydrate solution to obtain a material E, adjusting the pH value of the material E to 4.0, adding the material D, and stirring at room temperature for 20 hours to obtain a second slurry; the proportioning ratio of the sodium hydroxide solution, the aluminum chloride hexahydrate and the material D is 10mL:0.26mg:1g.
Preparation of a composite ceramic traction buckle:
(1) Mixing the first slurry and deionized water, wet-grinding for 4 hours by using zirconia beads, drying for 4 hours at 100 ℃, grinding, granulating, drying, and screening by using a 80-mesh screen to obtain first powder; the mass ratio of the first slurry to the deionized water to the zirconia beads is 1.5:1:1, a step of;
(2) Mixing the second slurry, zirconia powder and deionized water, wet-grinding for 6 hours by using zirconia beads, drying at 100 ℃ for 5 hours, grinding, granulating, drying, screening by a 60-mesh screen, screening the granules passing through the screen by a 80-mesh screen, and taking the granules left on the 80-mesh screen to obtain second powder; the mass ratio of the second slurry to the zirconia powder to the deionized water to the zirconia beads is 1.2:0.5:1:1, a step of;
(3) Uniformly paving the first powder in a die to obtain a first powder layer, uniformly paving the second powder on the first powder layer, and applying 10MPa pressure to maintain the pressure for 1min for compression molding to obtain a ceramic green body; the mass ratio of the first powder to the second powder is 75:45;
(5) And firing the preform at 1650 ℃ for 6 hours, and cooling to room temperature to obtain the composite ceramic traction buckle.
Performance testing
Flexural strength testing was performed according to standard GB/T4741-1999;
fracture toughness testing was performed according to standard GB/T23806-2009;
porosity testing was performed according to standard GB/T25995-2010;
the ceramic buttons produced in examples 1-4 and comparative examples 1-5 were tested for flexural strength and fracture toughness according to the above criteria, and the test results are shown in Table 1 below.
TABLE 1
As can be seen from table 1:
the comparative example 1 was inferior in toughness due to the absence of the second slurry in the preparation process, and the possible reason is that the porosity was greatly reduced, resulting in poor dispersion effect under stress, resulting in a significant decrease in fracture resistance of the prepared ceramic traction buckle as compared with example 1;
comparative example 2, in which no addition of the first slurry resulted in poor toughness, probably because no recoating occurred during the secondary firing, resulting in increased porosity and decreased density of the ceramic towing buckle, resulting in a ceramic towing buckle produced with less toughness than example 1;
comparative example 3, in which no material D was added during the preparation process, resulted in poor toughness, probably because the porosity of the prepared ceramic pulling buckle was reduced to result in a decrease in fracture resistance, but the presence of alumina moderately increased the fracture resistance of the ceramic pulling buckle;
The comparative example 4 only undergoes once low-temperature sintering in the preparation process, so that the density of the ceramic traction buckle is greatly reduced, and the fracture resistance of the ceramic traction buckle is reduced;
the ceramic traction buckle is further expanded by only once high-temperature sintering in the preparation process, so that the fracture resistance of the ceramic traction buckle is reduced.
The present invention is not limited to the above embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present invention.
Claims (10)
1. The preparation method of the composite ceramic traction buckle is characterized by comprising the following steps of:
(1) Mixing the first slurry with deionized water, ball milling, drying, grinding, granulating, drying, and sieving to obtain first powder;
(2) Mixing and ball milling the second slurry, zirconia powder and deionized water, drying, grinding and granulating, drying and sieving to obtain second powder;
(3) Uniformly paving the first powder in a die to obtain a first powder layer, uniformly paving the second powder on the first powder layer, and performing compression molding to obtain a ceramic green body;
(4) Firing the ceramic green body at 1150-1250 ℃ for 2-3h, and cooling to 80-100 ℃ to obtain a preform;
(5) Firing the preform at 1650-1700 ℃ for 4-6h, and cooling to room temperature to obtain the composite ceramic traction buckle;
wherein:
the preparation of the first slurry in step (1) comprises the following steps;
mixing and stirring a dispersing agent and deionized water for 20-30min, adding zirconia powder, performing ultrasonic dispersion for 20-30min to obtain a dispersion liquid, adding ammonia water to adjust the pH of the dispersion liquid to 8-12, and stirring for 2-3h to obtain the first slurry;
the preparation of the second slurry in step (2) comprises the following steps:
(21) Weighing montmorillonite, grinding, sieving, adding deionized water, stirring, standing, collecting upper suspension, centrifuging, and collecting solid phase to obtain material A;
(22) Mixing the material A, sodium chloride and deionized water, performing temperature control reaction, performing centrifugal separation, taking a solid phase, washing with water, and drying to obtain a material B;
(23) Mixing the material B with deionized water, stirring for 2-3h, adding octadecyl trimethyl ammonium chloride for temperature control reaction, filtering after the reaction is finished, washing, and drying to obtain a material C;
(24) Mixing the material C and isophorone diisocyanate in a reaction kettle, performing ultrasonic dispersion at 80 ℃ for 1-2 hours, adding polytetrahydrofuran ether glycol under the condition of introducing nitrogen, stirring, adding 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide and dibutyltin dilaurate, performing temperature control reaction, adding acetone, performing temperature control reaction continuously, adding triethylamine and deionized water after the reaction is finished, and stirring to obtain a material D;
(25) And mixing and stirring a sodium hydroxide solution and an aluminum trichloride hexahydrate solution to obtain a material E, adjusting the pH value of the material E to be 4.0-4.2, adding the material D, and stirring at room temperature for 20-30h to obtain the second slurry.
2. The method for preparing the composite ceramic traction buckle according to claim 1, wherein in the step (1), the ball milling means wet milling for 4-6 hours by using zirconia beads, and the mass ratio of the first slurry, deionized water and zirconia beads is 1.5-2.5:1:1, a step of; the sieving refers to sieving by using a 80-100 mesh sieve;
In the step (2), the ball milling refers to wet milling for 6-8 hours by using zirconia beads, wherein the mass ratio of the second slurry to the zirconia powder to the deionized water to the zirconia beads is 1.2-1.8:0.5-0.6:1:1, a step of; the sieving refers to sieving with a 60-mesh sieve, sieving the granules passing through the sieve with an 80-mesh sieve, and taking the granules left on the 80-mesh sieve;
in the step (3), the pressing forming refers to the forming by applying pressure of 10-12MPa for maintaining the pressure for 1-2 min; the mass ratio of the first powder to the second powder is 75-80:45-65.
3. The method for preparing a composite ceramic traction buckle according to claim 1, wherein in the preparation of the first slurry in the step (1), the mass ratio of the dispersant, deionized water and zirconia powder is 3.5-11.1:100:75-85.
4. The method for manufacturing a composite ceramic traction buckle according to claim 1, wherein in the step (21), the proportioning ratio of montmorillonite and deionized water is 100-200g:3-4L; the stirring time is 6-8h, and the standing time is 12-14h.
5. The method for preparing a composite ceramic traction buckle according to claim 1, wherein in the step (22), the mass ratio of the material a to sodium chloride to deionized water is 1-1.5:1-2:10-12; the temperature control reaction is carried out at 60-65 ℃ for 5-7h, and the temperature of drying is 100 ℃.
6. The method for preparing the composite ceramic traction buckle according to claim 1, wherein in the step (23), the mass ratio of the material B to deionized water to octadecyl trimethyl ammonium chloride is 2-3:10-12:0.5-0.8; the temperature control reaction is carried out at 80 ℃ for 5-6 hours.
7. The method for preparing a composite ceramic traction buckle according to claim 1, wherein in the step (24), the mass ratio of the material C, isophorone diisocyanate, polytetrahydrofuran ether glycol, 1, 4-butanediol, dimethylolpropionic acid, castor oil, 2-hydroxy-N, N-dimethylacetamide, dibutyltin dilaurate, acetone, triethylamine and deionized water is 1-1.5:0.5-0.6:0.8-1:0.2-0.4:0.08-0.1:0.05-0.08:0.04-0.06:0.02-0.03:5-10:0.5-0.6:10; the first temperature control reaction is carried out for 2-3 hours under the oil bath condition of 80 ℃; the second temperature control reaction is carried out for 30-40min under the condition of 35 ℃ oil bath.
8. The method for preparing a composite ceramic traction buckle according to claim 1, wherein in the step (25), the proportioning ratio of the sodium hydroxide solution, the aluminum trichloride hexahydrate and the material D is 10-20mL:0.26-0.27mg:1g.
9. The method for manufacturing a composite ceramic traction buckle according to claim 1, wherein in the preparation of the first slurry in the step (1), the dispersant is any one of ammonium polyacrylate, ammonium citrate, sodium hexametaphosphate and polyethylene glycol.
10. A composite ceramic traction buckle made by the method of any one of claims 1-9.
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