CN103086603B - Colored glass ceramic for manufacturing dental prosthesis and preparation method for colored glass ceramic - Google Patents

Colored glass ceramic for manufacturing dental prosthesis and preparation method for colored glass ceramic Download PDF

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CN103086603B
CN103086603B CN201210575426.0A CN201210575426A CN103086603B CN 103086603 B CN103086603 B CN 103086603B CN 201210575426 A CN201210575426 A CN 201210575426A CN 103086603 B CN103086603 B CN 103086603B
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look
zirconium
colored glass
dental prosthesis
colorant
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CN103086603A (en
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陈吉华
袁坤
王富
高婧
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Fourth Military Medical University FMMU
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Fourth Military Medical University FMMU
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Abstract

The invention relates to a ceramic for a dental prosthesis, and discloses a colored glass ceramic for manufacturing the dental prosthesis and a preparation method for the colored glass ceramic. By adopting the colored glass ceramic, under the condition that the requirements on mechanical property of a dental glass ceramic are met, 16 colors of a Vitapan Classical color board which is most frequently used in dentistry can be obtained. The colored glass ceramic for manufacturing the dental prosthesis is characterized by comprising the following components in percentage by mass: 98.5 to 99.85 percent of basic component and 0.15 to 1.5 percent of pigment component, wherein the basic component comprises the following components in percentage by mass: 56 to 59 percent of SiO2, 28 to 30 percent of Li2CO3, 3.7 to 4.0 percent of K2CO3, 2.7 to 3.0 percent of Al2O3, 2.3 to 2.4 percent of ZrO2, 1.5 to 1.6 percent of CeO2 and 2.5 to 3.0 percent of P2O5; and the pigment component comprises zirconium praseodymium yellow, zirconium iron pink or zirconium vanadium blue, or any combination thereof.

Description

A kind of colored glass pottery for making dental prosthesis and preparation method thereof
Technical field
The present invention relates to dental prosthesis pottery, particularly a kind of colored glass pottery for making dental prosthesis and preparation method thereof.
Background technology
Stupalith is because of its good biological safety and aesthetic property, and the application in field, oral cavity is more and more extensive, and has become emphasis and the focus of Oral Repair area research.Dental porcelain mainly comprises: feldspathic china, glass-ceramic, alumina ceramics and zirconium oxide porcelain.
Feldspathic china is low brilliant ceramic material, and its crystalline component is few, structurally closer to glass.The dental case permeability made with this kind of pottery is high, have good aesthetic property, but its flexural strength is usually lower, can only be used as finishing material or for making inlay and veneer of anterior tooth.Add white garnet, mica etc. can carry out toughness reinforcing to this kind of material, but toughness reinforcing after material intensity improve limited, be still confined to make inlay, labial teeth leaf-comb and veneer.
Alumina-ceramic and zirconia ceramics are the dental porcelains that physical strength is the highest, but its optical property is poor, pure aluminum oxide and zirconium oxide porcelain present opaque white, light transmission is little, be used for the making of the stratum basale of all kinds of dummy, the dummy aesthetic property made is poor with emulation property, is not suitable for the aesthetic orthopaedics for labial teeth.
Glass-ceramic is that it has concentrated the feature of pottery and glass by host glass by the obtained crystalline phase of controlling crystallizing and the equally distributed polycrystalline solids of glassy phase.Separate out crystalline phase by thermal treatment process, the strength of materials and toughness are improved; In addition, because glass-ceramic contains the glassy phase of certain content, possessing outstanding semi-transparent characteristic, farthest can reproduce color and luster and the light transmission features of natural teeth, is the preferred material of labial teeth aesthetic orthopaedics.Increasing glass-ceramic product by Application and Development in succession in Oral Repair field.But, substrate porcelain (core porcelain) color category of current Dental Glass Ceramics is less, color as IPS e.max substrate porcelain only has 3 ~ 5 kinds, and the color category of clinical conventional dentistry color board is more than 16 kinds, therefore, there is the problem inconsistent with the color of dentistry color board in the dummy made of the substrate porcelain of current commercial glass-ceramic, need dye when usually making to it.
Summary of the invention
The object of the present invention is to provide a kind of colored glass pottery for making dental prosthesis and preparation method thereof, when meeting Dental Glass Ceramics mechanical property requirements, 16 kinds of colors of the most frequently used Vitapan Classical color board of dentistry can be obtained.
To achieve these goals, the present invention is achieved by the following technical solutions.
Technical scheme one:
A kind of colored glass pottery for making dental prosthesis, it is characterized in that, comprising mass percent is the basal component of 98.5 ~ 99.85% and the colorant component of 0.15 ~ 1.5%; The mass percent of described basal component: the SiO of 56 ~ 59% 2, the Li of 28 ~ 30% 2cO 3, the K of 3.7 ~ 4.0% 2cO 3, the Al of 2.7 ~ 3.0% 2o 3, the ZrO of 2.3 ~ 2.4% 2, the CeO of 1.5 ~ 1.6% 2, and the P of 2.5 ~ 3.0% 2o 5; Described colorant component comprises zirconium praseodymium yellow, zirconium iron pink or zirconium vanadium blue, or their arbitrary combination.
In technique scheme, preferably, the mass percent of described colorant component is less than 1.0%.
Preferably, corresponding Vitapan Classical color board 16 kinds of colors, the mass percent of zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue three kinds of colorants is as following table:
Color notation Zirconium praseodymium yellow (wt%) Zirconium iron pink (wt%) Zirconium vanadium blue (wt%)
A1 0.13~0.28 0.03~0.09 0.01~0.05
A2 0.30~0.42 0.06~0.13 0.02~0.07
A3 0.44~0.56 0.10~0.17 0.04~0.09
A3.5 0.57~0.66 0.12~0.19 0.05~0.11
A4 0.67~0.90 0.13~0.25 0.06~0.14
B1 0.15~0.28 0.02~0.06 0.01~0.04
B2 0.30~0.44 0.04~0.09 0.02~0.06
B3 0.46~0.69 0.07~0.14 0.03~0.09
B4 0.70~0.90 0.10~0.18 0.05~0.11
C1 0.17~0.29 0.05~0.11 0.05~0.11
C2 0.30~0.44 0.08~0.15 0.08~0.15
C3 0.45~0.56 0.12~0.19 0.12~0.19
C4 0.57~0.76 0.15~0.25 0.15~0.25
D2 0.18~0.30 0.05~0.11 0.04~0.10
D3 0.32~0.59 0.10~0.20 0.08~0.17
D4 0.37~0.60 0.07~0.21 0.06~0.15
Preferably, A look in corresponding Vitapan Classical color board 16 kinds of colors, the mass ratio of the zirconium praseodymium yellow in its colorant component, zirconium iron pink, zirconium vanadium blue is 4.5:1.2:0.7; Corresponding its A1 look, A2 look, A3 look, A3.5 look, A4 look, the mass percent of colorant component is respectively: A1, and 0.3%; A2,0.5%; A3,0.7%; A3.5,0.85%; A4,1.0%.
Preferably, B look in corresponding Vitapan Classical color board 16 kinds of colors, the mass ratio of the zirconium praseodymium yellow in its colorant component, zirconium iron pink, zirconium vanadium blue is 5:1:0.6; Corresponding its B1 look, B2 look, B3 look, B4 look, the mass percent of colorant component is respectively: B1, and 0.3%; B2,0.5%; B3,0.75%; B4,1.0%.
Preferably, C look in corresponding Vitapan Classical color board 16 kinds of colors, the mass ratio of the zirconium praseodymium yellow in its colorant component, zirconium iron pink, zirconium vanadium blue is 4:1.3:1.2; Corresponding its C1 look, C2 look, C3 look, C4 look, the mass percent of colorant component is respectively: C1, and 0.4%; C2,0.6%; C3,0.8%; C4,1.0%.
Preferably, D2 and D3 look in corresponding Vitapan Classical color board 16 kinds of colors, the mass ratio of the zirconium praseodymium yellow in its colorant component, zirconium iron pink, zirconium vanadium blue is 4:1.4:1.1; Itself D2 and D3 look corresponding, the mass percent of colorant component is respectively: D2, and 0.4%; D3,0.6%.
Preferably, D4 look in corresponding Vitapan Classical color board 16 kinds of colors, the mass ratio of the zirconium praseodymium yellow in its colorant component, zirconium iron pink, zirconium vanadium blue is 5:1.1:1; Its D4 look corresponding, the mass percent of colorant component is 0.7%.
Technical scheme two:
The preparation method of the above-mentioned colored glass pottery for making dental prosthesis, is characterized in that, comprise the following steps:
Basal component and colorant component is taken according to mass percent.Basal component is poured in ball grinder, add dehydrated alcohol, wet ball grinding, mix post-drying, obtain mixed powder; Pour in quartz crucible by mixed powder again, 1400 ~ 1500 DEG C of melting 1.5 ~ 2h, then pour in deionized water by molten slurry, cold quenching, obtain glass particle; Glass particle is placed in agate jar, ball milling, dry, obtain glass powder; Again colorant and glass powder are placed in agate jar, ball milling, mixing, dry, obtain colored glass powder; Finally, colored glass powder is put into prefabricated flask cold isostatic compaction, and the base substrate after shaping carries out two-part crystallization and thermal treatment.
In technique scheme, described two-part crystallization and thermal treatment is 700 DEG C/5h and 900 DEG C/5h.
The color matching method of the glass-ceramic for making dental prosthesis of the present invention, can prepare the glass-ceramic possessing dentistry Vitapan Classical color board 16 kinds of colors, and the total content of its colorant component zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue is less than 1.0wt%.Add 1.0wt% colorant to the thing phase composite of glass-ceramic, microtexture and 3 curved intensity without impact.The three-point bending strength of the glass-ceramic after painted is (310MPa), meets dental porcelain ISO required standard.In addition, the glass-ceramic after painted, while acquisition high-mechanical property, still can keep good semipermeability.
Accompanying drawing explanation
Below in conjunction with accompanying drawing and concrete body embodiment, the present invention is described in further details.
Fig. 1 is not for adding colorant, adding the scanning electron microscope (SEM) photograph of the glass-ceramic of 1.0wt% monochrome and colour mixture colorant (zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue mass ratio are 10:3:3).
Fig. 2 is not for adding colorant, adding X-ray diffraction analysis (XRD) figure of the glass-ceramic of 1.0wt% monochrome and colour mixture colorant (zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue mass ratio are 10:3:3).
Fig. 3 is the colored glass pottery of embodiment 2 preparation and the shade guide teeth figure of dentistry Vitapan Classical color board 16 look.
Fig. 4 is the colored glass pottery of embodiment 3 preparation and the shade guide teeth figure of dentistry Vitapan Classical color board 16 look.
Fig. 5 is the colored glass pottery of embodiment 4 preparation and the shade guide teeth figure of dentistry Vitapan Classical color board 16 look.
Fig. 6 is the colored glass pottery of embodiment 5 preparation and the shade guide teeth figure of dentistry Vitapan Classical color board 16 look.
Embodiment
Embodiment 1
Take according to mass ratio: the SiO of 58.0% 2, the Li of 29.0% 2cO 3, the K of 3.7% 2cO 3, the Al of 2.8% 2o 3, the ZrO of 2.4% 2, the CeO of 1.5% 2, the P of 2.6% 2o 5500g is amounted to for subsequent use as batching.
By the SiO taken 2, Li 2cO 3, K 2cO 3, Al 2o 3, ZrO 2, CeO 2, P 2o 5pour in ball grinder, add 500ml dehydrated alcohol, wet ball grinding 8h, puts into baking oven after mixing, and dries 24h, obtains mixed powder for 80 DEG C.
Quartz crucible is placed in resistance furnace preheating, resistance furnace is with after 10 DEG C/min ramp to 1480 DEG C, and poured into by mixed powder in the quartz crucible of preheating, found 2h at 1480 DEG C, the molten slurry after melting is poured into rapidly in deionized water, and cold quenching, obtains glass particle.The glass particle obtained is placed in agate jar, adds 500ml dehydrated alcohol ball milling 12h, dry, cross 120 mesh sieves, get minus mesh, obtain glass powder.
Before zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue three kinds of colorants use with 10% hydrochloric acid in 80 DEG C of pickling 30min, then use washed with de-ionized water in supersonic cleaning machine, until pH value is 7.
Not add colorant, interpolation 1.0wt% monochrome and colour mixture colorant (zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue mass ratio are for 10:3:3) for grouping.Do not add colorant group, take 3g glass powder.Add 1.0wt% colorant group, take 2.97g glass powder and 0.03g colorant.Each group of glass powder and colorant are placed in agate jar respectively, ball milling 2h, mixing.Add 3mL deionized water in colored glass powder after mixing, and load prefabricated flask (cylindrical mold cavity, diameter 13mm), cold isostatic compaction under 250MPa pressure, form base substrate.Carry out crystallization and thermal treatment to above-mentioned base substrate, be warming up to 700 DEG C from room temperature, 700 DEG C of insulations, after 5 hours, are warming up to 900 DEG C, are incubated 5 hours, temperature rise rate 10 DEG C/min.Base substrate furnace cooling after crystallization completes, be prepared into corresponding glass-ceramic, X-ray diffraction analysis (XRD) figure of composition graphs 1 to be the scanning electron microscope (SEM) photograph of the glass-ceramic of not adding colorant, adding the monochromatic and colour mixture colorant (zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue mass ratio are 10:3:3) of 1.0wt% and Fig. 2 be the glass-ceramic of not adding colorant, adding 1.0wt% monochrome and colour mixture colorant (zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue mass ratio are 10:3:3), and three-point bending strength and transparency (TP value) analysis are carried out to it, result is as following table.
Three-point bending strength (MPa) Transparency (TP value)
Do not add colorant 312±22 a 21.0±0.4 a
Add 1.0wt% zirconium praseodymium yellow 301±16 a 29.7±0.6 b
Add 1.0wt% zirconium iron pink 306±27 a 14.0±0.4 c
Add 1.0wt% zirconium vanadium blue 299±22 a 13.0±0.3 d
Add 1.0wt% colour mixture 315±19 a 15.7±0.7 e
*same letter shows no difference of science of statistics between group (p > 0.05)
Add the microtexture of colorant to the glass-ceramic for making dental prosthesis of the present invention of 1.0wt%, thing phase composite and three-point bending strength not make significant difference.Prepared colored glass pottery, when meeting Dental Glass Ceramics mechanical property requirements, still can keep good semipermeability.
Embodiment 2
Take according to mass percent: the SiO of 58.0% 2, the Li of 29.0% 2cO 3, the K of 3.7% 2cO 3, the Al of 2.8% 2o 3, the ZrO of 2.4% 2, the CeO of 1.5% 2, the P of 2.6% 2o 5500g is amounted to for subsequent use as batching.
By the SiO taken 2, Li 2cO 3, K 2cO 3, Al 2o 3, ZrO 2, CeO 2, P 2o 5pour in ball grinder, add 500ml dehydrated alcohol, wet ball grinding 8h, puts into baking oven after mixing, and dries 24h, obtains mixed powder for 80 DEG C.
Quartz crucible is placed in resistance furnace preheating, resistance furnace is with after 10 DEG C/min ramp to 1480 DEG C, and poured into by mixed powder in the quartz crucible of preheating, found 2h at 1480 DEG C, the molten slurry after melting is poured into rapidly in deionized water, and cold quenching, obtains glass particle.The glass particle obtained is placed in agate jar, adds 500ml dehydrated alcohol ball milling 12h, dry, cross 120 mesh sieves, get minus mesh, obtain glass powder.
Before zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue three kinds of colorants use with 10% hydrochloric acid in 80 DEG C of pickling 30min, then use washed with de-ionized water in supersonic cleaning machine, until pH value is 7.According to Vitapan Classical color board 16 look color formulas, take glass powder and colorant amounts to 2g, the concrete percent mass proportioning of each colorant sees the following form:
Color notation Zirconium praseodymium yellow (wt%) Zirconium iron pink (wt%) Zirconium vanadium blue (wt%) Glass powder (wt%)
A1 0.21 0.06 0.03 99.70
A2 0.35 0.09 0.05 99.51
A3 0.49 0.13 0.08 99.30
A3.5 0.60 0.16 0.09 99.15
A4 0.70 0.19 0.11 99.00
B1 0.23 0.05 0.03 99.69
B2 0.38 0.08 0.05 99.49
B3 0.57 0.11 0.07 99.25
B4 0.76 0.15 0.09 99.00
C1 0.25 0.08 0.07 99.60
C2 0.37 0.12 0.11 99.40
C3 0.49 0.16 0.15 99.20
C4 0.61 0.20 0.19 99.00
D2 0.25 0.09 0.07 99.59
D3 0.37 0.13 0.10 99.40
D4 0.49 0.11 0.10 99.30
Each group of glass powder and colorant are placed in agate jar respectively, ball milling 2h, mixing.Add 2mL deionized water in colored glass powder after mixing, and load prefabricated flask (cylindrical mold cavity, diameter 13mm), cold isostatic compaction under 250MPa pressure, form base substrate.Carry out crystallization and thermal treatment to above-mentioned base substrate, be warming up to 700 DEG C from room temperature, 700 DEG C of insulations, after 5 hours, are warming up to 900 DEG C, are incubated 5 hours, temperature rise rate 10 DEG C/min.Base substrate furnace cooling after crystallization completes, namely completes the preparation being applied to the colored glass pottery making dental prosthesis mutually.
Glass-ceramic (as shown in Figure 3) after painted by above-mentioned preparation method obtains the color close with dentistry VitapanClassical color board, and each porcelain block is 4.7 with the average color difference between corresponding shade guide teeth, is less than clinically to accept threshold.
Embodiment 3
Take according to mass ratio: the SiO of 58.0% 2, the Li of 29.0% 2cO 3, the K of 3.7% 2cO 3, the Al of 2.8% 2o 3, the ZrO of 2.4% 2, the CeO of 1.5% 2, the P of 2.6% 2o 5500g is amounted to for subsequent use as batching.
By the SiO taken 2, Li 2cO 3, K 2cO 3, Al 2o 3, ZrO 2, CeO 2, P 2o 5pour in ball grinder, add 500ml dehydrated alcohol, wet ball grinding 8h, puts into baking oven after mixing, and dries 24h, obtains mixed powder for 80 DEG C.
Quartz crucible is placed in resistance furnace preheating, resistance furnace is with after 10 DEG C/min ramp to 1480 DEG C, and poured into by mixed powder in the quartz crucible of preheating, found 2h at 1480 DEG C, the molten slurry after melting is poured into rapidly in deionized water, and cold quenching, obtains glass particle.The glass particle obtained is placed in agate jar, adds 500ml dehydrated alcohol ball milling 12h, dry, cross 120 mesh sieves, get minus mesh, obtain glass powder.
Before zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue three kinds of colorants use with 10% hydrochloric acid in 80 DEG C of pickling 30min, then use washed with de-ionized water in supersonic cleaning machine, until pH value is 7.According to Vitapan Classical color board 16 look color formulas, take glass powder and colorant amounts to 2g, the concrete percent mass proportioning of each colorant sees the following form:
Color notation Zirconium praseodymium yellow (wt%) Zirconium iron pink (wt%) Zirconium vanadium blue (wt%) Glass powder (wt%)
A1 0.22 0.05 0.02 99.71
A2 0.37 0.09 0.04 99.50
A3 0.52 0.12 0.06 99.30
A3.5 0.63 0.15 0.07 99.15
A4 0.74 0.18 0.08 99.00
B1 0.24 0.04 0.02 99.70
B2 0.40 0.07 0.04 99.49
B3 0.60 0.10 0.06 99.24
B4 0.80 0.13 0.07 99.00
C1 0.24 0.08 0.08 99.60
C2 0.35 0.12 0.12 99.41
C3 0.47 0.16 0.16 99.21
C4 0.58 0.21 0.21 99.00
D2 0.24 0.08 0.07 99.61
D3 0.37 0.12 0.11 99.40
D4 0.43 0.16 0.11 99.30
Each group of glass powder and colorant are placed in agate jar respectively, ball milling 2h, mixing.Add 2mL deionized water in colored glass powder after mixing, and load prefabricated flask (cylindrical mold cavity, diameter 13mm), cold isostatic compaction under 250MPa pressure, form base substrate.Carry out crystallization and thermal treatment to above-mentioned base substrate, be warming up to 700 DEG C from room temperature, 700 DEG C of insulations, after 5 hours, are warming up to 900 DEG C, are incubated 5 hours, temperature rise rate 10 DEG C/min.Base substrate furnace cooling after crystallization completes, namely completes the preparation being applied to the colored glass pottery making dental prosthesis mutually.
Glass-ceramic (as shown in Figure 4) after painted by above-mentioned preparation method obtains the color close with dentistry VitapanClassical color board, and each porcelain block is 5.3 with the average color difference between corresponding shade guide teeth, is less than clinically to accept threshold.
Embodiment 4
Take according to mass ratio: the SiO of 58.0% 2, the Li of 29.0% 2cO 3, the K of 3.7% 2cO 3, the Al of 2.8% 2o 3, the ZrO of 2.4% 2, the CeO of 1.5% 2, the P of 2.6% 2o 5500g is amounted to for subsequent use as batching.
By the SiO taken 2, Li 2cO 3, K 2cO 3, Al 2o 3, ZrO 2, CeO 2, P 2o 5pour in ball grinder, add 500ml dehydrated alcohol, wet ball grinding 8h, puts into baking oven after mixing, and dries 24h, obtains mixed powder for 80 DEG C.
Quartz crucible is placed in resistance furnace preheating, resistance furnace is with after 10 DEG C/min ramp to 1480 DEG C, and poured into by mixed powder in the quartz crucible of preheating, found 2h at 1480 DEG C, the molten slurry after melting is poured into rapidly in deionized water, and cold quenching, obtains glass particle.The glass particle obtained is placed in agate jar, adds 500ml dehydrated alcohol ball milling 12h, dry, cross 120 mesh sieves, get minus mesh, obtain glass powder.
Before zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue three kinds of colorants use with 10% hydrochloric acid in 80 DEG C of pickling 30min, then use washed with de-ionized water in supersonic cleaning machine, until pH value is 7.According to Vitapan Classical color board 16 look color formulas, take glass powder and colorant amounts to 2g, the concrete percent mass proportioning of each colorant sees the following form:
Color notation Zirconium praseodymium yellow (wt%) Zirconium iron pink (wt%) Zirconium vanadium blue (wt%) Glass powder (wt%)
A1 0.23 0.05 0.02 99.70
A2 0.39 0.08 0.04 99.49
A3 0.54 0.11 0.05 99.30
A3.5 0.66 0.13 0.06 99.15
A4 0.77 0.16 0.07 99.00
B1 0.25 0.04 0.02 99.69
B2 0.41 0.06 0.03 99.50
B3 0.61 0.09 0.05 99.25
B4 0.81 0.12 0.06 99.01
C1 0.25 0.08 0.08 99.59
C2 0.37 0.12 0.12 99.39
C3 0.50 0.15 0.15 99.20
C4 0.62 0.19 0.19 99.00
D2 0.25 0.08 0.07 99.60
D3 0.38 0.12 0.10 99.40
D4 0.44 0.15 0.11 99.30
Each group of glass powder and colorant are placed in agate jar respectively, ball milling 2h, mixing.Add 2mL deionized water in colored glass powder after mixing, and load prefabricated flask (cylindrical mold cavity, diameter 13mm), cold isostatic compaction under 250MPa pressure, form base substrate.Carry out crystallization and thermal treatment to above-mentioned base substrate, be warming up to 700 DEG C from room temperature, 700 DEG C of insulations, after 5 hours, are warming up to 900 DEG C, are incubated 5 hours, temperature rise rate 10 DEG C/min.Namely base substrate furnace cooling after crystallization completes completes the preparation being applied to the colored glass pottery making dental prosthesis mutually.
Glass-ceramic (as shown in Figure 5) after painted by above-mentioned preparation method obtains the color close with dentistry VitapanClassical color board, and each porcelain block is 6.2 with the average color difference between corresponding shade guide teeth, is less than clinically to accept threshold.
Embodiment 5
Take according to mass ratio: the SiO of 58.0% 2, the Li of 29.0% 2cO 3, the K of 3.7% 2cO 3, the Al of 2.8% 2o 3, the ZrO of 2.4% 2, the CeO of 1.5% 2, the P of 2.6% 2o 5500g is amounted to for subsequent use as batching.
By the SiO taken 2, Li 2cO 3, K 2cO 3, Al 2o 3, ZrO 2, CeO 2, P 2o 5pour in ball grinder, add 500ml dehydrated alcohol, wet ball grinding 8h, puts into baking oven after mixing, and dries 24h, obtains mixed powder for 80 DEG C.
Quartz crucible is placed in resistance furnace preheating, resistance furnace is with after 10 DEG C/min ramp to 1480 DEG C, and poured into by mixed powder in the quartz crucible of preheating, found 2h at 1480 DEG C, the molten slurry after melting is poured into rapidly in deionized water, and cold quenching, obtains glass particle.The glass particle obtained is placed in agate jar, adds 500ml dehydrated alcohol ball milling 12h, dry, cross 120 mesh sieves, get minus mesh, obtain glass powder.
Before zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue three kinds of colorants use with 10% hydrochloric acid in 80 DEG C of pickling 30min, then use washed with de-ionized water in supersonic cleaning machine, until pH value is 7.According to Vitapan Classical color board 16 look color formulas, take glass powder and colorant amounts to 2g, the concrete percent mass proportioning of each colorant sees the following form:
Color notation Zirconium praseodymium yellow (wt%) Zirconium iron pink (wt%) Zirconium vanadium blue (wt%) Glass powder (wt%)
A1 0.22 0.06 0.02 99.70
A2 0.37 0.10 0.04 99.49
A3 0.52 0.13 0.05 99.30
A3.5 0.63 0.16 0.06 99.15
A4 0.73 0.19 0.08 99.00
B1 0.24 0.05 0.02 99.69
B2 0.40 0.08 0.03 99.49
B3 0.60 0.11 0.05 99.24
B4 0.79 0.14 0.07 99.00
C1 0.26 0.07 0.07 99.60
C2 0.39 0.11 0.11 99.39
C3 0.52 0.14 0.14 99.20
C4 0.64 0.18 0.18 99.00
D2 0.26 0.08 0.06 99.60
D3 0.39 0.12 0.10 99.39
D4 0.49 0.12 0.10 99.29
Each group of glass powder and colorant are placed in agate jar respectively, ball milling 2h, mixing.Add 2mL deionized water in colored glass powder after mixing, and load prefabricated flask (cylindrical mold cavity, diameter 13mm), cold isostatic compaction under 250MPa pressure, form base substrate.Carry out crystallization and thermal treatment to above-mentioned base substrate, be warming up to 700 DEG C from room temperature, 700 DEG C of insulations, after 5 hours, are warming up to 900 DEG C, are incubated 5 hours, temperature rise rate 10 DEG C/min.Base substrate furnace cooling after crystallization completes, namely completes the preparation being applied to the colored glass pottery making dental prosthesis mutually.
Lithium bisilicate glass-ceramic (as shown in Figure 6) after painted by above-mentioned preparation method obtains the color close with dentistry Vitapan Classical color board, and each porcelain block is 6.6 with the average color difference between corresponding shade guide teeth, is less than clinically to accept threshold.
Above content is in conjunction with concrete preferred implementation further description made for the present invention; can not assert that the specific embodiment of the present invention is only limitted to this; for general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; some simple deduction or replace can also be made, all should be considered as belonging to the present invention by submitted to claims determination scope of patent protection.

Claims (8)

1. one kind for make dental prosthesis colored glass pottery, it is characterized in that, comprising mass percent is the basal component of 98.5 ~ 99.85% and the colorant component of 0.15 ~ 1.5%; The mass percent of described basal component: the SiO of 56 ~ 59% 2, the Li of 28 ~ 30% 2cO 3, the K of 3.7 ~ 4.0% 2cO 3, the Al of 2.7 ~ 3.0% 2o 3, the ZrO of 2.3 ~ 2.4% 2, the CeO of 1.5 ~ 1.6% 2, and the P of 2.5 ~ 3.0% 2o 5; Described colorant component comprises zirconium praseodymium yellow, zirconium iron pink or zirconium vanadium blue, or their arbitrary combination; Corresponding Vitapan Classical color board 16 kinds of colors, the mass percent of described zirconium praseodymium yellow, zirconium iron pink, zirconium vanadium blue three kinds of colorants is as following table:
Color notation Zirconium praseodymium yellow (wt%) Zirconium iron pink (wt%) Zirconium vanadium blue (wt%) A1 0.13~0.28 0.03~0.09 0.01~0.05 A2 0.30~0.42 0.06~0.13 0.02~0.07 A3 0.44~0.56 0.10~0.17 0.04~0.09 A3.5 0.57~0.66 0.12~0.19 0.05~0.11 A4 0.67~0.90 0.13~0.25 0.06~0.14 B1 0.15~0.28 0.02~0.06 0.01~0.04 B2 0.30~0.44 0.04~0.09 0.02~0.06 B3 0.46~0.69 0.07~0.14 0.03~0.09 B4 0.70~0.90 0.10~0.18 0.05~0.11 C1 0.17~0.29 0.05~0.11 0.05~0.11 C2 0.30~0.44 0.08~0.15 0.08~0.15 C3 0.45~0.56 0.12~0.19 0.12~0.19 C4 0.57~0.76 0.15~0.25 0.15~0.25 D2 0.18~0.30 0.05~0.11 0.04~0.10
D3 0.32~0.59 0.10~0.20 0.08~0.17 D4 0.37~0.60 0.07~0.21 0.06~0.15
2. the colored glass pottery for making dental prosthesis according to claim 1, it is characterized in that, A1 look, A2 look, A3 look, A3.5 look, A4 look in corresponding Vitapan Classical color board 16 kinds of colors, the mass ratio of the zirconium praseodymium yellow in its colorant component, zirconium iron pink, zirconium vanadium blue is 4.5:1.2:0.7; Corresponding its A1 look, A2 look, A3 look, A3.5 look, A4 look, the mass percent of colorant component is respectively: A1, and 0.3%; A2,0.5%; A3,0.7%; A3.5,0.85%; A4,1.0%.
3. the colored glass pottery for making dental prosthesis according to claim 1, it is characterized in that, B1 look, B2 look, B3 look, B4 look in corresponding Vitapan Classical color board 16 kinds of colors, the mass ratio of the zirconium praseodymium yellow in its colorant component, zirconium iron pink, zirconium vanadium blue is 5:1:0.6; Corresponding its B1 look, B2 look, B3 look, B4 look, the mass percent of colorant component is respectively: B1, and 0.3%; B2,0.5%; B3,0.75%; B4,1.0%.
4. the colored glass pottery for making dental prosthesis according to claim 1, it is characterized in that, C1 look, C2 look, C3 look, C4 look in corresponding Vitapan Classical color board 16 kinds of colors, the mass ratio of the zirconium praseodymium yellow in its colorant component, zirconium iron pink, zirconium vanadium blue is 4:1.3:1.2; Corresponding its C1 look, C2 look, C3 look, C4 look, the mass percent of colorant component is respectively: C1, and 0.4%; C2,0.6%; C3,0.8%; C4,1.0%.
5. the colored glass pottery for making dental prosthesis according to claim 1, it is characterized in that, D2 and D3 look in corresponding Vitapan Classical color board 16 kinds of colors, the mass ratio of the zirconium praseodymium yellow in its colorant component, zirconium iron pink, zirconium vanadium blue is 4:1.4:1.1; Itself D2 and D3 look corresponding, the mass percent of colorant component is respectively: D2, and 0.4%; D3,0.6%.
6. the colored glass pottery for making dental prosthesis according to claim 1, it is characterized in that, D4 look in corresponding Vitapan Classical color board 16 kinds of colors, the mass ratio of the zirconium praseodymium yellow in its colorant component, zirconium iron pink, zirconium vanadium blue is 5:1.1:1; Its D4 look corresponding, the mass percent of colorant component is 0.7%.
7. the preparation method of the colored glass pottery for making dental prosthesis according to claim 1, is characterized in that, comprise the following steps:
Take basal component and colorant component according to mass percent, basal component is poured in ball grinder, add dehydrated alcohol, wet ball grinding, mix post-drying, obtain mixed powder; Pour in quartz crucible by mixed powder again, 1400 ~ 1500 DEG C of melting 1.5 ~ 2h, then pour in deionized water by molten slurry, cold quenching, obtain glass particle; Glass particle is placed in agate jar, ball milling, dry, obtain glass powder; Again colorant and glass powder are placed in agate jar, ball milling, mixing, dry, obtain colored glass powder; Finally, colored glass powder is put into prefabricated flask cold isostatic compaction, and the base substrate after shaping carries out two-part crystallization and thermal treatment.
8. the preparation method of the colored glass pottery for making dental prosthesis according to claim 7, is characterized in that, described two-part crystallization and thermal treatment is 700 DEG C/5h and 900 DEG C/5h.
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