CN110040965A - A kind of machinable ceramic material and preparation method thereof - Google Patents
A kind of machinable ceramic material and preparation method thereof Download PDFInfo
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- CN110040965A CN110040965A CN201910252783.5A CN201910252783A CN110040965A CN 110040965 A CN110040965 A CN 110040965A CN 201910252783 A CN201910252783 A CN 201910252783A CN 110040965 A CN110040965 A CN 110040965A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
Abstract
A kind of machinable ceramic material of the present invention and preparation method thereof, the material include mass percent be 70-90% glass powder, mass percent be 5-20% nano diatomite and mass percent be 1-10% ZrO2；The glass powder includes the following components'mass percentage: the MgF of 15-30%2, 5-20% P2O5, 5-15% K2O, the Al of 5-10%2O3(tiny balloon) and 25-40%SiO2The glass powder of composition.It is the method for modifying agent that the material, which takes addition nano diatomite, and nano diatomite is dispersed in glass phase, plays fiber self toughening humidification.Machinable ceramic material sintering temperature of the present invention is low, and bending strength, fracture toughness improve.
Description
Technical field
A kind of machinable ceramic material of the present invention and preparation method thereof, belongs to medical material tech field.
Background technique
The development of dental material and its processing technology has pushed the raising at full speed of dental care level.It is new in the latest 20 years
Type Post-core material, binder material, full ceramic restoration material are gradually promoted come in clinical application, with the progress of these technologies
Also bigger opportunity is provided to the development of CAD/CAM, also proposes more urgent requirement in clinical popularization for it.And it can cut
The research for cutting material then obtains many important development under the strength curbing function of this demand.
CAD/CAM system does not require nothing more than the machinability and certain mechanical strength of ceramic material, and prior one is wanted
Seeking Truth also needs material that can imitate the translucence of natural teeth, exactly because machinable ceramic is provided with these features and gets over
To be more widely used in CAD/CAM system by the chair of oral cavity.
The had optical characteristics of All-ceramic material is the unrivaled aesthetic advantage of other materials, therefore is gradually obtained most wide
General clinical application, even if All-ceramic material equally occupies great specific gravity in the dummy of traditional manufacturing technique.Such as
During planting body is repaired, the ratio of All-ceramic restoration is continuously increased, this reflects its aesthetics of the all-ceramic prosthesis of conventional machining process
It can be affirmed fully by people, while its mechanical strength can satisfy the needs of clinical application completely.Harder is for kind
It is found in the retrospective analysis for the all-ceramic prosthesis research that implant is supported, the dummy of the full porcelain fixed bridge of implant-supported its 5 years
Dummy survival rate be up to 81.4% to 95.6%, and 5 years dummy survival rates of the full porcelain leaf-comb of implant-supported are then
It is close to 100%, 95% credibility interval CI:92.4-100；5 years dummy survival rate reports of full porcelain fixed bridge dummy of full denture
Road is the survival rate same nearly 100% of full porcelain leaf-comb dummy between 72.2% to 100%.To implant-supported form in report
The percentage that case statistics show that fixed bridge and leaf-comb collapse porcelain is respectively 0.43 (95% CI:0.06-3.06) and 3.61
(95% CI:2.05-6.36), these are statistics indicate that the all-ceramic prosthesis of conventional machining process its mechanical strength completely can be with
Meet clinical application needs
Report that more ceramic material has Al at present2O3, mica, ZrO2And the ceramic materials such as glass-infiltrated ceramic.But these are made pottery
Ceramic material there are sintering temperatures it is high, intensity and toughness are relatively low the problems such as.
Summary of the invention
The present invention overcomes the shortcomings of the prior art, and the technical problem to be solved is that provide a kind of machinable ceramic material
Material and preparation method thereof, the material sintering temperature is low, intensity is high, toughness is high.
In order to solve the above technical problems, the technical scheme adopted by the invention is that:
A kind of machinable ceramic material, including mass percent be 70-90% glass powder, mass percent be 5-20% nanometer
The ZrO that diatomite and mass percent are 1-10%2；
The glass powder includes the following components'mass percentage: the MgF of 15-30%2, 5-20% P2O5, 5-15% K2O、5-
10% Al2O3(tiny balloon) and 25-40% SiO2The glass powder of composition.
Preferably, a kind of machinable ceramic material, which is characterized in that including mass percent be 70-90% glass powder,
The ZrO that the nano diatomite and mass percent that mass percent is 5-20% are 1-10%2；
The glass powder includes the following components'mass percentage: the MgF of 15-25%2, 15-20% P2O5, 10-15% K2O、
The Al of 5-10%2O3(tiny balloon) and 30-35% SiO2The glass powder of composition.
A kind of preparation method of machinable ceramic material, comprising the following steps:
Step 1) is according to mass percent by the MgF of 15-30%2, 5-20% P2O5, 5-15% K2O, the Al of 5-10%2O3And 25-
40% SiO2Ingredient ball milling is carried out, the hole 120-250/cm is crossed2Sub-sieve is warming up to 1100 DEG C, keeps the temperature 2-4 hours, melts water cooling,
It is ground up, sieved obtained glass powder；
The glass powder of 70-90%, mass percent are the nano diatomite and quality of 5-20% according to mass percent by step 2
Percentage is the ZrO of 1-10%2Second batch is carried out, ingredient A is obtained；
Ingredient A ball milling is crossed the hole 120-250/cm by step 3)2The binder of ingredient A mass percent 5-8% is added in sub-sieve
It is granulated, is pressed into green compact, be warming up to 400-500 DEG C and be warming up to 1000 DEG C of -1030 DEG C of heat preservations 1 hour again, ceramics are made after cooling
Material.
Preferably, Ball-milling Time is 4-6 hours in the step 1), and ball-milling medium is the zirconia ball that diameter is 1mm.
Preferably, heating rate is 5-10 DEG C/min in the step 1), and optimum temperature rise rate is 7 DEG C/min.
Preferably, the mistake to heat up in the step 3) is known as being heated to 400-500 DEG C by the heating rate of 2 DEG C/min, then
1000 DEG C -1030 DEG C are heated to by the heating rate of 10 DEG C/min.
Preferably, binder is polyvinyl alcohol or paraffin in the step 3).
Glass ceramics is the composite material of crystal and glass ingredient, performance by two kinds of components property and the common shadow of quantity
It rings.The intensity of glass ceramics, be mainly sintered in the type that precipitates crystal, the size of crystal grain, the number of crystal phase and glass
Quality and quantity are influenced.The type precipitated crystal, the size of crystal grain, crystal phase number receive glass matrix, nucleation crystallization
The joint effects of the factors such as agent, additive and sintering process, formula and technique complement each other, joint effect glass ceramics
Performance.
About preparation machinable ceramic material method, specifically, first, early period glass powder preparation process in, no
Same firing process, the glass powder performance prepared are different.Second, the tiny balloon Al in glass frit component2O3Add with the later period
The nano diatomite added not only makes to obtain higher stream before nucleation and crystallization occurs inside Fluorosilicic mica glass ceramic material
Dynamic property is conducive to form the microstructure of stable homogeneous inside glass ceramics and obtains higher mechanical strength, because of nucleus shape
It is related with the high granular of nano material and active state at temperature.Third, nano diatomite porous framework structure and hollow micro-
Ball Al2O3It is easy to absorb energy, and glass phase is made to form glass fibre, play fiber self toughening humidification.4th, individually
Diatomite ceramics, individual aluminium oxide ceramics and individual glass powder on sintering temperature, machinability, strength and toughness all without
Method reaches performance actually required.
This preparation method realizes the activeness and quietness of machinable ceramic, this preparation method consumption by control preparation process condition
Can be low, low in cost, with short production cycle, product quality repeatability is high.And large-scale high-accuracy sintering experiment furnace is not needed, is such as put
Electric plasma heating furnace or atmosphere hot pressing sintering furnace etc. are completed, and are effectively saved cost, and improve production efficiency.
Compared to the prior art the present invention has the advantages that
Fluorosilicic mica glass ceramics system's machinable ceramic has moderate sintering temperature, generally at 1100 DEG C or so, with excellent
Cutting ability and good biocompatibility, be applied to the department of stomatology repair field ideal material.
The present invention selects this system, and taking addition nano diatomite is the method for modifying agent, is lower than its sintering temperature
1100 DEG C and bending strength, fracture toughness raising.Its activeness and quietness dominant mechanism:
First, nano diatomite itself has porous frame structure, and the presence of these micropores has conducive to material structure stress
Release；Nano diatomite is dispersed in glass phase, when external force makes material micro-crack occur or expands original crack
Zhan Shi, it can prevent its crack propagation；Porous framework structure is easy that glass phase is made to form glass fibre, plays fiber self toughening
Humidification.
Second, glass powder formula in tiny balloon Al2O3It on the one hand is the nucleation crystallization agent of glass ceramics, remaining is more
Stress can be absorbed in the material by dissipating, and have the function that activeness and quietness.
Third, the ZrO added in inventive formulation2, under stress, tetragonal phase ZrO2Crystal transition is generated, becomes single
Monoclinic phase ZrO2In the process, energy is absorbed along with the variation of volume and shape, reduces the concentration of crack tip stress, prevents to split
Line extension, to make ceramic material property activeness and quietness.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described, it is clear that and described embodiment is a part of the embodiments of the present invention, and
The embodiment being not all of.
Embodiment 1
According to ratio ingredient described in the following table 1, ball milling 6 hours on the ball mill that revolving speed is 400r/min, in the common baking of 3.3kw
In 100 DEG C of dryings in case, 250 holes/cm is crossed2Sub-sieve is warming up to 1100 DEG C with 5 DEG C/min, and heat preservation 2 is small at 1100 DEG C
When, water cooling is melted, grinding is sieved and glass powder is made.
Table 1
Second batch is carried out, according to 90% glass powder, 5% nano diatomite and 5%ZrO2Relationship between quality uniformly mix, add from
Sub- water is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill in revolving speed28wt% is added in sub-sieve
Paraffin is granulated, and is pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then add by the heating rate of 10 DEG C/min
Heat keeps the temperature 1 hour, ceramic dielectric is made after cooling to 1000 DEG C of firings.
The test result of above-described embodiment mechanical property is detailed in the following table 2.
Table 2
Embodiment 2
According to ratio ingredient described in the following table 3, ball milling 4 hours on the ball mill that revolving speed is 400r/min, in the common baking of 3.3kw
In 100 DEG C of dryings in case, 250 holes/cm is crossed2Sub-sieve is warming up to 1100 DEG C with 7 DEG C/min, and heat preservation 2 is small at 1100 DEG C
When, water cooling is melted, grinding is sieved and glass powder is made.
Table 3
Second batch is carried out, according to 85% glass powder, 10% nano diatomite and 5%ZrO2Relationship between quality uniformly mix, add from
Sub- water is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill in revolving speed28wt% is added in sub-sieve
Paraffin is granulated, and is pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then add by the heating rate of 10 DEG C/min
Heat keeps the temperature 1 hour, ceramic dielectric is made after cooling to 1010 DEG C of firings.
The test result of above-described embodiment mechanical property is detailed in the following table 4.
Table 4
Embodiment 3
According to ratio ingredient described in the following table 5, ball milling 4 hours on the ball mill that revolving speed is 400r/min, in the common baking of 3.3kw
In 100 DEG C of dryings in case, 250 holes/cm is crossed2Sub-sieve is warming up to 1100 DEG C with 7 DEG C/min, and heat preservation 3 is small at 1100 DEG C
When, water cooling is melted, grinding is sieved and glass powder is made.
Table 5
Second batch is carried out, according to 80% glass powder, 15% nano diatomite and 5%ZrO2Relationship between quality uniformly mix, add from
Sub- water is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill in revolving speed28wt% is added in sub-sieve
Paraffin is granulated, and is pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then add by the heating rate of 10 DEG C/min
Heat keeps the temperature 1 hour, ceramic dielectric is made after cooling to 1020 DEG C of firings.
The test result of above-described embodiment mechanical property is detailed in the following table 6.
Table 6
Embodiment 4
According to ratio ingredient described in the following table 7, ball milling 5 hours on the ball mill that revolving speed is 400r/min, in the common baking of 3.3kw
In 100 DEG C of dryings in case, 250 holes/cm is crossed2Sub-sieve is warming up to 1100 DEG C with 10 DEG C/min, and heat preservation 4 is small at 1100 DEG C
When, water cooling is melted, grinding is sieved and glass powder is made.
Table 7
Second batch is carried out, according to 70% glass powder, 20% nano diatomite and 10%ZrO2Relationship between quality uniformly mix, add
Ionized water is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill in revolving speed2Sub-sieve is added
8wt% paraffin is granulated, and is pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then by the heating speed of 10 DEG C/min
Rate is heated to 1030 DEG C of firings, keeps the temperature 1 hour, and ceramic dielectric is made after cooling.
The test result of above-described embodiment mechanical property is detailed in the following table 8.
Table 8
Embodiment 5
A kind of machinable ceramic material, by 83% glass powder of mass percent, 16% nano diatomite of mass percent and quality hundred
Divide and compares 1%ZrO2Composition；
The glass powder includes the following components'mass percentage:
30% MgF2, 5% P2O5, 15% K2O, 10% Al2O3(tiny balloon) and 40% SiO2The glass powder of composition.
Embodiment 6
A kind of machinable ceramic material, by 87% glass powder of mass percent, 10% nano diatomite of mass percent and quality hundred
Divide and compares 3%ZrO2Composition；The glass powder includes the following components'mass percentage:
30% MgF2, 20% P2O5, 5% K2O, 10% Al2O3(tiny balloon) and 35% SiO2The glass powder of composition.
Test method and detection device used in the present invention are as follows:
1, the test of bending strength
Three-point bending survey is carried out to sample using Changchun experimental machine research CSS-55300 type almighty test machine produced
Examination, sample are 25mm × 5mm × 4mm strip, every group of at least three sample.Loading speed is 0.4mm/min, and span is
15mm.Bending strength σbCalculation formula are as follows:
Wherein, maximum load when P is sample fracture, L is span, and b is specimen width, and h is specimen height.
2, the test of fracture toughness
Three-point bending survey is carried out to sample using Changchun experimental machine research CSS-55300 type almighty test machine produced
Examination, sample are 25mm × 2.5mm × 5mm strip, and the midpoint of each test specimen prepares deep 2.5 mm, the transverse direction of wide 0.3 mm
Every group of at least three sample of notch.Loading speed is 0.05mm/min, span 15mm.Fracture toughness KICCalculation formula are as follows:
Wherein, S, B, w, a respectively represent the load span of test sample, thickness, the dimensional parameters in width and middle part crack；
P is the concentrfated load of middle part load；For the shape correlation coefficients of different test test specimens.This sample calculating formula are as follows:
3, the test of microhardness
Impression is prepared on Vickers.Ram load 88.2N, dwell time 15s, makes c >=2.5a.The calculating of Vickers hardness
Formula are as follows:
Wherein, Hv is Vickers hardness, and P is ram load, and c is impression center to crack tip length, and 2a is impression diagonal line length
Degree.
The present invention is explained in detail above in conjunction with embodiment, but the present invention is not limited to above-described embodiments, at this
Field those of ordinary skill within the scope of knowledge, can also make various changes without departing from the purpose of the present invention
Change.
Claims (7)
1. a kind of machinable ceramic material, which is characterized in that glass powder, mass percent including mass percent for 70-90%
The ZrO that nano diatomite and mass percent for 5-20% are 1-10%2；
The glass powder includes the following components'mass percentage:
The MgF of 15-30%2, 5-20% P2O5, 5-15% K2O, the Al of 5-10%2O3(tiny balloon) and 25-40% SiO2Composition
Glass powder.
2. a kind of machinable ceramic material according to claim 1, which is characterized in that including mass percent be 70-90%
Glass powder, mass percent be 5-20% nano diatomite and mass percent be 1-10% ZrO2；
The glass powder includes the following components'mass percentage:
The MgF of 15-25%2, 15-20% P2O5, 10-15% K2O, the Al of 5-10%2O3(tiny balloon) and 30-35% SiO2Group
At glass powder.
3. a kind of preparation method of machinable ceramic material, which comprises the following steps:
Step 1) is according to mass percent by the MgF of 15-30%2, 5-20% P2O5, 5-15% K2O, the Al of 5-10%2O3And 25-
40% SiO2Ingredient ball milling is carried out, the hole 120-250/cm is crossed2Sub-sieve is warming up to 1100 DEG C, keeps the temperature 2-4 hours, melts water cooling,
It is ground up, sieved obtained glass powder；
The glass powder of 70-90%, mass percent are the nano diatomite and quality of 5-20% according to mass percent by step 2
Percentage is the ZrO of 1-10%2Second batch is carried out, ingredient A is obtained；
Ingredient A ball milling is crossed the hole 120-250/cm by step 3)2Sub-sieve, the binder that ingredient A mass percent 5-8% is added are made
Grain, is pressed into green compact, is warming up to 400-500 DEG C and is warming up to 1000 DEG C of -1030 DEG C of heat preservations 1 hour again, ceramic material is made after cooling
Material.
4. a kind of preparation method of machinable ceramic material according to claim 3, which is characterized in that in the step 1)
Ball-milling Time is 4-6 hours, and ball-milling medium is the zirconia ball that diameter is 1mm.
5. a kind of preparation method of machinable ceramic material according to claim 3, which is characterized in that in the step 1)
Heating rate is 5-10 DEG C/min.
6. a kind of preparation method of machinable ceramic material according to claim 3, which is characterized in that in the step 3)
Heating rate is to be heated to 400-500 DEG C by the heating rate of 2 DEG C/min, then be heated to by the heating rate of 10 DEG C/min
1000℃-1030℃。
7. a kind of preparation method of machinable ceramic material according to claim 3, which is characterized in that in the step 3)
Binder is polyvinyl alcohol or paraffin.
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| CN113158491A (en) * | 2021-05-14 | 2021-07-23 | 南京工程学院 | Ceramic special-shaped micropore damage strength limit judging method and device, computer equipment and storage medium |
| CN114380504A (en) * | 2022-01-29 | 2022-04-22 | 山东国瓷功能材料股份有限公司 | Microcrystalline glass composite material and preparation method and application thereof |
| CN114507071A (en) * | 2022-03-05 | 2022-05-17 | 太原理工大学 | High-strength ceramic dielectric material and preparation method thereof |
| CN114890680A (en) * | 2022-06-10 | 2022-08-12 | 杨晓战 | Preparation method of glass ceramic capable of being machined and glass ceramic device |
| CN115124246A (en) * | 2022-06-10 | 2022-09-30 | 杨晓战 | High bending strength zirconia microcrystalline glass and machinable ceramic product |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113158491A (en) * | 2021-05-14 | 2021-07-23 | 南京工程学院 | Ceramic special-shaped micropore damage strength limit judging method and device, computer equipment and storage medium |
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| CN114890680A (en) * | 2022-06-10 | 2022-08-12 | 杨晓战 | Preparation method of glass ceramic capable of being machined and glass ceramic device |
| CN115124246A (en) * | 2022-06-10 | 2022-09-30 | 杨晓战 | High bending strength zirconia microcrystalline glass and machinable ceramic product |
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