CN108578250A - A kind of resin penetration silicate composite material and its preparation and application - Google Patents
A kind of resin penetration silicate composite material and its preparation and application Download PDFInfo
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- CN108578250A CN108578250A CN201810426620.XA CN201810426620A CN108578250A CN 108578250 A CN108578250 A CN 108578250A CN 201810426620 A CN201810426620 A CN 201810426620A CN 108578250 A CN108578250 A CN 108578250A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/887—Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
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Abstract
The present invention relates to a kind of resin penetration silicate composite materials, and by the component including resin and glass phase silicate, cured reaction is made in the presence of a curing agent；Wherein, the resin includes Bisphenol A-glycidyl Methacrylate and tetraethylene-glycol dimethylacrylate.The invention further relates to a kind of preparation methods of resin penetration silicate composite material, it prepares porous ceramics block by controlling sintering temperature and soaking time, then by vacuum capillarity by resin penetration to porous ceramics block, then cured formation silicate/resin dual-network structure.Resin penetration silicate composite material provided by the invention has both higher mechanical property and aesthetic properties, has huge potentiality to be exploited and vast market prospect in gear division reparation application aspect.
Description
Technical field
The invention belongs to gear division reparation technical field of composite materials, and in particular to a kind of resin penetration silicate composite wood
Material and its preparation and application.
Background technology
Survey data shows, the populations of dental caries is suffered from there are about 600,000,000, there are about 80% with each in teenager by China at present
Kind dental disorder, average every patient are related to 2~3 teeth.With the enhancing of mankind's self health consciousness, to Dental Erosion
Demand shows a rising trend.It is not suffering from the population of dental disorder, tooth is repaiied for aesthetic consideration (smile's transformation)
Multiple demand also increases severely with day.As the improvement of people's living standards, the requirement of the aesthetic properties to materials of bone tissue
It is higher and higher.
Current main repair materials have：Metal alloy, full porcelain, ceramic deposited metal and compound resin.Metal have compared with
High mechanical property, but its aesthetic properties and biocompatibility are poor.Some countries of Europe clearly forbid argental mercury in recent years
The materials such as alloy are used for Dental Erosion.Full ceramic restoration material has higher mechanical property and aesthetic properties, but its machinability
It is poor, it is more sensitive to crackle, the energy force difference of tensile stress is born, these disadvantages are easy to cause the initial failure of All-ceramic restoration, pottery
The excessively high hardness of porcelain also can cause to wear to primary tooth.Ceramic deposited metal attempts to combine the advantage of metal and ceramics, but heat
The main reason for mismatch of conductance and modulus is its initial failure.In recent years, with raising, the holding required aesthetic properties
The enhancing of primary tooth consciousness and going deep into for minimally invasive reparation idea, Compound resin repair material is increasingly becoming main reparation material
Material.It is that compound resin is applied to dental prosthetic to reduce shrinkage stress, prolong the service life, improve mechanical property and biocompatibility
The significant challenge of material.
It is a marked improvement of gear division reparation using polymer matrix composites.Bowen R L report epoxy resin and
Silica dioxide granule is combined as gear division reparation (Bowen R L.Use of epoxy resins in restorative
materials.J Dent Res,1956,35(3):360-369).It is a kind of important in its subsequent work (US3179623)
Monomer Bis-GMA be developed, which becomes the skeleton of gear division reparation composite material, behind gear division reparation composite wood
It is constantly used in material.
Materials of bone tissue is classified according to its repair mode, can be divided into direct repair materials and be repaired material indirectly
Material, this kind of criteria for classification is mainly for polymer matrix composites.Due to the lower mechanical property of direct repair composite material and gather
It closes and shrinks, currently, indirect repair composite material has become the first choice of dentist and patient.With CAD and calculating
The development of machine auxiliary manufacture, indirect repair composite material have occurred that huge change.CAD and computer
Auxiliary manufacture and the combination of indirect repair composite material are more and more closer, and therefore, indirect repair composite material is also known as CAD/CAM
Block.
In terms of mechanical property, reach it is suitable with dentine be teeth repairing material industry common recognition.Enamel and dentine
Some mechanical properties be listed in table 1.It is Vita companies that mesh first two, which is widely used general commercial materials of bone tissue,
The Lava Ultimate products of Vita Enamic products and 3M ESPE companies.The bending strength of Vita Enamic be 150~
160MPa, also larger with the bending strength gap of dentine, the bending strength of 3M ESPE is (204 ± 19) MPa, although
Close to the lower limit of dentine bending strength, but also certain gap.The elasticity modulus of Vita Enamic is 30GPa, and value is
More than dentine；The elasticity modulus of Lava Ultimate is (12.77 ± 0.99) GPa, lower than dentine.Vita
The Vickers hardness of Enamic is 2.5GPa, and the Vickers hardness of 3M ESPE Lava Ultimate is (1.15 ± 0.13) GPa,
Value is between dentine and enamel.
Some mechanical properties of 1 dentine of table and enamel
In terms of aesthetic properties, realize that gear division reparation composite material translucence or the transparency have vital meaning.One
Aspect, translucent is presented at primary enamel margin, and translucent gear division reparation composite material and enamel are more close.
On the other hand, translucent gear division reparation composite material makes coloring be more prone to, convenient for according to the primary color of teeth of different people
It is coloured.The color and luster of Vita Enamic and Lava Ultimate are close with primary tooth, but its transparency is to be improved.
Therefore, presently, there are the problem of be to be badly in need of researching and developing a kind of resin penetration silicate composite material and its preparation side
Method and its application in gear division reparation.
Invention content
The technical problem to be solved by the present invention is to solve the above shortcomings of the prior art and to provide a kind of resin penetration silicic acid
Salt composite material and preparation method and application.The present inventor is carried out in gear division reparation with technical field of composite materials
Experimental study extensively and profoundly finds the porous ceramics block partially sintered by control sintering temperature and soaking time preparation,
Then by vacuum capillarity by resin penetration to the porous ceramics block partially sintered, then cured reaction, form silicon
Hydrochlorate/resin dual-network structure.Composite material prepared by the method for the present invention has been effectively combined the advantage of resin and ceramics, together
When have higher mechanical property and aesthetic properties.
For this purpose, first aspect present invention provides a kind of resin penetration silicate composite material, by including resin and glass
Cured reaction is made the component of glass phase silicate in the presence of a curing agent；Wherein, the resin includes the double metering systems of bisphenol-A
Acid glycidyl ester (Bis-GMA) and tetraethylene-glycol dimethylacrylate (TEGDMA).
In some specific embodiments, the mass ratio of the resin, glass phase silicate and curing agent is 1:
(0.75-4.0):(0.005-0.02)。
In some preferred embodiments, the Bisphenol A-glycidyl Methacrylate and tetraethylene-glycol
The mass ratio of dimethylacrylate is (1-4):1, more preferably (1-2):1.
In some specific embodiments, the glass phase silicate is selected from aerosil, alumina silicate, alumina silicate
It is one or more in sodium, sodium metasilicate, potassium silicate, magnesium silicate, calcium silicates, barium silicate and zirconium silicate.
In other specific embodiments, the curing agent is selected from benzoyl peroxide, dicumyl peroxide and mistake
It is one or more in Methyl Ethyl Ketone Oxidation.
Second aspect of the present invention provides a kind of preparation method of the composite material described according to a first aspect of the present invention, packet
It includes：
Step A will carry out the powder obtained after ball milling, drying process through molding, sintering processes, system to glass phase silicate
Obtain porous ceramic block；
Step B permeates the resin containing curing agent into porous ceramics block, and the sufficient block of resin penetration is made；
Resin penetration silicate composite material is made in the cured processing of the sufficient block of resin penetration by step C.
In some specific embodiments, in step, the abrasive material of the ball-milling treatment is zirconia ball；The ball
The speed of mill processing is 100-350r/min；The time of the ball-milling treatment is 12-24h；The temperature of the drying process is 50-
90℃。
According to some specific embodiments, in step, the forming processes include compression molding and isostatic cool pressing.
According to some specific embodiments, the pressure of the compression molding is 2-4MPa, dwell time 1-3min.
According in other specific embodiments, the pressure of the isostatic cool pressing is 150-220MPa, and the dwell time is
1.5-2min。
In the present invention, the size of isostatic cool pressing pressure can influence the hardness and modulus of composite material.Control isostatic cool pressing
The pressure of power can make the hardness for the composite material being finally prepared and modulus higher.
According to some specific embodiments, in step, the sintering processes carry out at a temperature of being gradually increased,
The heating rate of the sintering processes is 5-10 DEG C/min；The holding temperature of the sintering processes is 550-850 DEG C, the sintering
The soaking time of processing is 1min-2h.
In the present invention, sintering temperature and soaking time can influence porosity, pore structure to finally influence composite wood
The mechanical property of material.Control sintering can make the porosity of finally formed composite material low with soaking time, and hole pattern becomes
In mellow and full, therefore the elasticity modulus for the composite material being prepared and hardness are higher.
According to some specific embodiments, in step, when the caking property of powder is poor, then in the molding of powder
Further include step D before processing, binder and powder are subjected to mixed processing.
In some preferred embodiments, the mass ratio of the binder and powder is (0.01-0.1):1.
In other preferred embodiments, the mass concentration of the binder is 0.5-10wt%.
In other preferred embodiments, the binder is selected from polyvinyl alcohol water solution, amidin, paste
It is one or more in the aqueous solution of smart aqueous solution and carboxymethyl cellulose.
According to some specific embodiments, in stepb, the infiltration is (- 0.01)-(- 0.1) MPa's in pressure
It is carried out under vacuum condition；The time of the infiltration is 1-48h.
According to some specific embodiments, in step C, the curing process is vacuum solidification；The vacuum solidification
Temperature be 70-110 DEG C；The time of the vacuum solidification is 8-16h.
In some preferred embodiments, in step C, the curing process at different temperature in two steps into
Row.For example, the curing process carries out in a low temperature of 70-90 DEG C (the case where comprising being equal to 90 DEG C) first, then (no 90
Including the case where equal to 90 DEG C) it carries out at a high temperature of -110 DEG C, the total time of two-stage cure processing is 8-16h.It is solid using substep
Change can improve curing degree.
In some specific embodiments, the preparation method of the resin penetration silicate composite material includes following step
Suddenly：
(1) by glass phase silicate and solvent according to 1:10 mass ratio mixing, is made solidliquid mixture；It is preferred that described molten
Agent is ethyl alcohol or deionized water；
(2) solidliquid mixture is injected in ball grinder and carries out ball-milling treatment, use zirconia ball for abrasive material, ball milling speed is
The powder after ball milling is made in 100-350r/min, Ball-milling Time 12-24h；
(3) powder after ball milling is dried to processing at 50-90 DEG C for 24 hours, the powder after being made dry；
(4) powder after drying is subjected to mixed processing with binder, the powder containing binder is made；The binder with
The mass ratio of powder after drying is (0.01-0.1):1；
(5) use compression molding die by the pressed by powder containing binder at green body, the pressure of compression molding is 2-4MPa,
Dwell time is 1-3min, is then demoulded, and the green body after compression molding is made；
(6) green body after compression molding is placed in progress isostatic cool pressing processing, the pressure of isostatic cool pressing in oil pressure environment is
The green body after isostatic cool pressing is made in 150-220MPa, dwell time 1.5-2min；
(7) porous ceramics block is sintered at a temperature of being gradually increased the green body after isostatic cool pressing into, heating rate is
5-10 DEG C/min, soaking time 1min-2h；Holding temperature is 550-850 DEG C；
(8) it is (1-4) to mass ratio:1 Bisphenol A-glycidyl Methacrylate and tetraethylene-glycol dimethyl
0.5wt%-2.0wt% is added in the resin compound of acrylate and (is based on Bisphenol A-glycidyl Methacrylate and three
The gross mass of contracting tetraethylene glycol dimethylacrylate) curing agent, be made the resin containing curing agent；
(9) by the resin penetration porous ceramics block containing curing agent, method is：It is previously implanted in a mold a certain amount of
Resin is advisable with 1/3 height of porous ceramics block, and in resin place porous ceramics block, osmotic pressure be (-
0.01) it-(- 0.1) is permeated under the vacuum environment of MPa, time of penetration 1-48h, until resin penetration is abundant, resin penetration is made
Sufficient block；
(10) the sufficient block of resin penetration is placed under 70-110 DEG C of vacuum condition and is cured, hardening time 8-16h,
Block after solidification obtained is resin penetration silicate composite material.
Third aspect present invention provides a kind of resin penetration silicate composite wood according to a first aspect of the present invention
The application of resin penetration silicate composite material prepared by material or according to a second aspect of the present invention the method in gear division reparation.
When resin penetration silicate composite material provided by the invention is used for gear division reparation, its surface need to be beaten
Grinding and polishing light processing.For example, with the table of the block (i.e. resin penetration silicate composite material) after the coarse sandpaper polishing solidification of 150 mesh
Face resin-rich layer, then polished with the fine sandpaper of 2000 mesh, and polish, gear division reparation resin penetration silicate composite wood is made
Material.
Unless otherwise specified, material therefor of the present invention, reagent can be obtained by commercial sources.
Unless otherwise specified, experimental method used in the present invention is this field conventional method.
Term " holding temperature " of the present invention refers to sintering temperature, also refers to heating final temperature.
Term " soaking time " of the present invention refers to the retention time at a sintering temperature.
Resin penetration silicate composite material provided by the invention and preparation method thereof has the following advantages that：
(1) preparation method of resin penetration silicate composite material provided by the invention is simple, and technological parameter is easily controllable；
(2) resin penetration silicate composite material provided by the invention have higher aesthetic properties, it is translucent with
The translucence of enamel margin is more closely, be convenient for being coloured according to the primary color of teeth of different people, and this is compound
Material can be realized from super translucent to milky continuous controllable adjustment；
(3) resin penetration silicate composite material provided by the invention has higher bending strength, fracture toughness, moderate
Hardness and modulus；
(4) resin penetration silicate composite material provided by the invention has huge exploitation in gear division reparation application aspect
Potentiality and vast market prospect.
Description of the drawings
Fig. 1 is the secondary electron figure of the burnishing surface of resin penetration silicate composite material prepared by the embodiment of the present invention 1.
Fig. 2 is the secondary electron figure of the section of resin penetration silicate composite material prepared by the embodiment of the present invention 1.
Fig. 3 is the backscattered electron figure of the burnishing surface of resin penetration silicate composite material prepared by the embodiment of the present invention 1.
Fig. 4 is the backscattered electron figure of the section of resin penetration silicate composite material prepared by the embodiment of the present invention 1.
Fig. 5 is the sample drawing of resin penetration silicate composite material prepared by the embodiment of the present invention 4.
Specific implementation mode
To keep the present invention easier to understand, below in conjunction with embodiment and attached drawing, the present invention will be described in detail, these realities
Apply example only serve it is illustrative, it is not limited to application range of the invention.
Using the AGS-X type instrument test bending strengths of Japanese Shimadzu Corporation's production in the present invention.Test condition is：Using
Three-point bending pattern, wide × height × span are 2mm × 2mm × 10mm, loading speed 0.5mm/min.It uses and receives in the present invention
Rice indentation equipment (MTS, XP, the U.S.) testing elastic modulus and hardness, compression distance 1000nm are kept for 4 seconds.
Embodiment
Embodiment 1
20g lagoriolites are weighed, are placed in ball grinder, alcohol and zirconia ball, rotating speed 250r/min, ball milling is added
24h.Solidliquid mixture after ball milling is poured into container, is placed into 70 DEG C of environment and dries, collect the powder.Utilize moulding press
It is green body by the pressed by powder, pressure 3MPa, dwell time 3min completely demould the green body.The green body that will be suppressed
It is placed in rubber membrane, the air in rubber membrane is extracted out using vacuum pumping, and is closed, be the cold etc. quiet of 220MPa using pressure
Pressure handles above-mentioned green body, dwell time 1.5min.The above-mentioned green body after isostatic cool pressing is taken out, is burnt in the environment of 550 DEG C
Knot, heating rate are 5 DEG C/min, soaking time 1min, and the porous ceramics block partially sintered is made.By the double methyl of bisphenol-A
Glycidyl acrylate is 1 in mass ratio with tetraethylene-glycol dimethylacrylate:1 is mixed, and 2h is stirred, will
2wt%'s (gross mass based on Bisphenol A-glycidyl Methacrylate Yu tetraethylene-glycol dimethylacrylate)
Benzoyl peroxide is added in above-mentioned mixed liquor and continues to stir 2h.Resin mixture liquor is injected in mold, liquid level is block
The 1/3 of body height.The above-mentioned lagoriolite block partially sintered is placed in one, is placed in vacuum environment, utilizes vacuum capillary
Infiltration resin is acted on, is kept for 24 hours, until porous ceramics block is saturated fully.The ceramic block of infiltration resin is placed on -0.1MPa
Vacuum drying oven in cure, solidification temperature be 70 DEG C, hardening time 16h, obtain resin penetration silicate composite material (tree
The mass ratio of fat, lagoriolite and benzoyl peroxide three is 1:4.0:0.02, wherein resin is bisphenol-A methacrylate
The general name of ethylene oxidic ester and tetraethylene-glycol dimethylacrylate).With the block after the coarse sandpaper polishing solidification of 150 mesh
Surface resin-rich layer, then with the fine sandpaper of 2000 mesh polish, be used in combination diamond polishing powder to polish, ultimately form for gear division
The resin penetration silicate composite material of reparation.
The secondary electron figure of burnishing surface of composite material prepared by the embodiment, the secondary electron figure of section, burnishing surface
The backscattered electron figure of backscattered electron figure and section difference is as shown in Figs 1-4.From figure 1 it appears that the composite material table
Face no marking has preferable polishing performance.From figure 2 it can be seen that the resin phase in the composite material is formed with ceramic phase
Good combination.From figure 3, it can be seen that the composite material has good polishing performance.Figure 4, it is seen that should
Resin phase in composite material can form good combination with ceramic phase.
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 2
The preparation method is the same as that of Example 1 for resin penetration silicate composite material, the difference is that, sintering temperature 600
℃。
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 3
The preparation method is the same as that of Example 1 for resin penetration silicate composite material, the difference is that, sintering temperature 650
℃。
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 4
The preparation method is the same as that of Example 1 for resin penetration silicate composite material, the difference is that, sintering temperature 700
℃。
The sample drawing of composite material prepared by the embodiment is as shown in Figure 5.From figure 5 it can be seen that the composite material is in
Existing milky, has good aesthetic properties.
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 5
The preparation method is the same as that of Example 1 for resin penetration silicate composite material, the difference is that, sintering temperature 750
℃。
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 6
The preparation method is the same as that of Example 1 for resin penetration silicate composite material, the difference is that, sintering temperature 800
℃。
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 7
The preparation method is the same as that of Example 1 for resin penetration silicate composite material, the difference is that, sintering temperature 850
℃。
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 8
The preparation method is the same as that of Example 1 for resin penetration silicate composite material, the difference is that, curing is：It is first
First cure 8h at 70 DEG C, then cures 8h at 110 DEG C.
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 9
The preparation method of resin penetration silicate composite material with embodiment 2, the difference is that, curing is：It is first
First cure 8h at 70 DEG C, then cures 8h at 110 DEG C.
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 10
The preparation method of resin penetration silicate composite material with embodiment 3, the difference is that, curing is：It is first
First cure 8h at 70 DEG C, then cures 8h at 110 DEG C.
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 11
The preparation method of resin penetration silicate composite material with embodiment 4, the difference is that, curing is：It is first
First cure 8h at 70 DEG C, then cures 8h at 110 DEG C.
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 12
The preparation method of resin penetration silicate composite material with embodiment 5, the difference is that, curing is：It is first
First cure 8h at 70 DEG C, then cures 8h at 110 DEG C.
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 13
The preparation method of resin penetration silicate composite material with embodiment 6, the difference is that, curing is：It is first
First cure 8h at 70 DEG C, then cures 8h at 110 DEG C.
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 14
The preparation method of resin penetration silicate composite material with embodiment 7, the difference is that, curing is：It is first
First cure 8h at 70 DEG C, then cures 8h at 110 DEG C.
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 15
The preparation method of resin penetration silicate composite material with embodiment 4, the difference is that, soaking time 2h.
The mechanical performance data of composite material prepared by the embodiment is shown in Table 1.
Embodiment 16
The preparation method is the same as that of Example 1 for resin penetration silicate composite material, the difference is that, the double methyl-props of bisphenol-A
The mass ratio of olefin(e) acid ethylene oxidic ester and tetraethylene-glycol dimethylacrylate is 2:1.
Embodiment 17
The preparation method is the same as that of Example 1 for resin penetration silicate composite material, the difference is that, the double methyl-props of bisphenol-A
The mass ratio of olefin(e) acid ethylene oxidic ester and tetraethylene-glycol dimethylacrylate is 3:1.
The mechanical property of 1 resin penetration silicate composite material of table
From table 1 it follows that resin penetration silicate composite material prepared by resin system using the present invention has
Good mechanical property (especially having higher elasticity modulus and hardness) and aesthetic properties, achieve preferable effect.
It should be noted that embodiment described above is only used for explaining the present invention, do not constitute to any of the present invention
Limitation.By referring to exemplary embodiments, invention has been described, it should be appreciated that word used in it is descriptive
With explanatory vocabulary, rather than limited vocabulary.The present invention can be made within the scope of the claims by regulation
Modification, and the present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it relates to
And specific method, material and embodiment, it is not intended that the present invention is limited to particular case disclosed in it, on the contrary, this hair
It is bright to can be extended to other all methods and applications with the same function.
Claims (11)
1. a kind of resin penetration silicate composite material is existed by the component including resin and glass phase silicate in curing agent
Under it is cured reaction be made；Wherein, the resin includes Bisphenol A-glycidyl Methacrylate and tetraethylene-glycol two
Methacrylate.
2. composite material according to claim 1, which is characterized in that the resin, glass phase silicate and curing agent
Mass ratio is 1:(0.75-4.0):(0.005-0.02)；
Preferably, the quality of the Bisphenol A-glycidyl Methacrylate and tetraethylene-glycol dimethylacrylate
Than for (1-4):1.
3. composite material according to claim 1 or 2, which is characterized in that the glass phase silicate is selected from gas phase dioxy
One kind or more in SiClx, alumina silicate, lagoriolite, sodium metasilicate, potassium silicate, magnesium silicate, calcium silicates, barium silicate and zirconium silicate
Kind；
The curing agent is one or more in benzoyl peroxide, dicumyl peroxide and methyl ethyl ketone peroxide.
4. a kind of preparation method according to any one of the claim 1-3 composite materials comprising：
Step A will carry out the powder obtained after ball milling, drying process through molding, sintering processes to glass phase silicate, be made more
Hole ceramic block；
Step B permeates the resin containing curing agent into porous ceramics block, and the sufficient block of resin penetration is made；
Resin penetration silicate composite material is made in the cured processing of the sufficient block of resin penetration by step C.
5. preparation method according to claim 4, which is characterized in that in step, the abrasive material of the ball-milling treatment is oxygen
Change zirconium ball；The speed of the ball-milling treatment is 100-350r/min；The time of the ball-milling treatment is 12-24h；
The temperature of the drying process is 50-90 DEG C.
6. preparation method according to claim 4 or 5, which is characterized in that in step, the forming processes include mould
Molded and isostatic cool pressing；
The pressure of the compression molding is 2-4MPa, dwell time 1-3min；
The pressure of the isostatic cool pressing is 150-220MPa, dwell time 1.5-2.0min.
7. according to the preparation method described in any one of claim 4-6, which is characterized in that in step, at the sintering
Reason carries out at a temperature of being gradually increased, and the heating rate of the sintering processes is 5-10 DEG C/min；The guarantor of the sintering processes
Temperature is 550-850 DEG C, and the soaking time of the sintering processes is 1min-2h.
8. according to the preparation method described in any one of claim 4-7, which is characterized in that in step, manage at the forming site
Before, further include step D, binder and powder are subjected to mixed processing；
It is preferred that the mass ratio of the binder and powder is (0.01-0.1):1；The mass concentration of the more preferable binder is
0.5-10wt%；The further preferred binder is selected from polyvinyl alcohol water solution, amidin, dextrin in aqueous solution and carboxylic first
It is one or more in base cellulose aqueous solution.
9. according to the preparation method described in any one of claim 4-8, which is characterized in that in stepb, the infiltration exists
It is carried out under the vacuum condition that pressure is (- 0.01)-(- 0.1) MPa；The time of the infiltration is 1-48h.
10. according to the preparation method described in any one of claim 4-9, which is characterized in that in step C, the solidification
Processing is vacuum solidification；The temperature of the vacuum solidification is 70-110 DEG C；The time of the vacuum solidification is 8-16h.
11. a kind of resin penetration silicate composite material according to any one of claim 1-3 is wanted according to right
Ask application of the resin penetration silicate composite material of any one of 4-10 the methods preparation in gear division reparation.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110028333A (en) * | 2019-03-06 | 2019-07-19 | 北京化工大学 | Gear division reparation resin penetration zero dimension/one-dimensional porous ceramic composite and preparation method thereof |
| CN112295871A (en) * | 2019-07-31 | 2021-02-02 | 共享智能铸造产业创新中心有限公司 | Technology for pressurizing and permeating reinforcer on surface of mould and container |
| CN114712250A (en) * | 2022-03-14 | 2022-07-08 | 华南理工大学 | Crown and bridge repairing ceramic with efficient anti-deformation streptococcus and preparation and application thereof |
| CN114732742A (en) * | 2022-03-14 | 2022-07-12 | 华南理工大学 | Efficient anti-deformation streptococcus aluminum sodium silicate/nano copper oxide composite ceramic and preparation and application thereof |
| CN115894001A (en) * | 2023-03-10 | 2023-04-04 | 湖南康纳新材料有限公司 | High-hardness wear-resistant resin-permeable ceramic composite material and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110028333A (en) * | 2019-03-06 | 2019-07-19 | 北京化工大学 | Gear division reparation resin penetration zero dimension/one-dimensional porous ceramic composite and preparation method thereof |
| CN112295871A (en) * | 2019-07-31 | 2021-02-02 | 共享智能铸造产业创新中心有限公司 | Technology for pressurizing and permeating reinforcer on surface of mould and container |
| CN114712250A (en) * | 2022-03-14 | 2022-07-08 | 华南理工大学 | Crown and bridge repairing ceramic with efficient anti-deformation streptococcus and preparation and application thereof |
| CN114732742A (en) * | 2022-03-14 | 2022-07-12 | 华南理工大学 | Efficient anti-deformation streptococcus aluminum sodium silicate/nano copper oxide composite ceramic and preparation and application thereof |
| CN115894001A (en) * | 2023-03-10 | 2023-04-04 | 湖南康纳新材料有限公司 | High-hardness wear-resistant resin-permeable ceramic composite material and preparation method and application thereof |
| CN115894001B (en) * | 2023-03-10 | 2023-05-09 | 湖南康纳新材料有限公司 | High-hardness wear-resistant resin-infiltrated ceramic composite material and preparation method and application thereof |
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| CN108578250B (en) | 2023-07-11 |
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