CN102153284B - Novel method for preparing lithium-based casting ceramic block - Google Patents

Novel method for preparing lithium-based casting ceramic block Download PDF

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Publication number
CN102153284B
CN102153284B CN2010106042724A CN201010604272A CN102153284B CN 102153284 B CN102153284 B CN 102153284B CN 2010106042724 A CN2010106042724 A CN 2010106042724A CN 201010604272 A CN201010604272 A CN 201010604272A CN 102153284 B CN102153284 B CN 102153284B
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porcelain
ratio
lithium
powder
weight
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CN102153284A (en
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朱伟凤
严庆云
李英春
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SHANGHAI UPCERA ORAL CAVITY TECHNOLOGY CO., LTD.
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Liaoning Upcera Biomaterial Co Ltd
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Abstract

The invention belongs to the technical field of a dental prosthesis material and particularly relates to a method for preparing a lithium-based casting ceramic block. The method comprises the following steps of carrying out melting on the raw material, carrying out water quenching on the molten raw material, drying the obtained product, carrying out ball milling, mixing the obtained powder and a coloring agent, carrying out isostatic pressing forming, carrying out crystallization heat treatment and obtaining the product. In the method, substrate glass powder only needs to be prepared in one step and a crucible does not need to be cleaned; a user dose not need to worry about the chromatic aberration caused by high temperature valence alternation of variable valence metal ions; products with different colors can be produced; the lithium-based casting ceramic block is uniform to color and has pure color; the forming process is easy to operate; the diversity of product sizes can be realized; and the production energy consumption is low and energy is saved, so as to save the production cost, thereby solving the energy problem.

Description

A kind of preparation method of lithium base casting porcelain porcelain piece
Technical field
The invention belongs to a kind of technical field of dental prosthetic material, relate in particular to a kind of preparation method of lithium base casting porcelain porcelain piece.
Background technology
Casting porcelain tooth full name is the castable ceramic complete crown, also claims full porcelain tooth.It is emerging in recent years complete crown dummy, is made by the new ceramic material that can cast.Produce the die of corona or end hat earlier with wax, the dewax that in the porcelain oven body of special use, heats up after the embedding in that finished product porcelain piece fusing back is cast in the die through pressure, obtains casting porcelain tooth after the cooling.The composition of porcelain is a lithium-based ceramic, and its intensity is high, has good transparence, and aesthetic is good, can be used for dental prosthetic materials such as inlay, veneer, labial teeth or backteeth leaf-comb, the preceding bridge of 3 units.
Because the difference of material, casting porcelain tooth and porcelain tooth have had essential different, the performance of following excellence occurred:
1, transparent: this is the porcelain impossible mission; Because hat is opaque in the metal; Need to hide metal base with opaque porcelain; Influence the transparency of dummy, making has tangible chalk look, pale, false after the porcelain beauty treatment, attractive in appearance in " black line " influence that neck portion more has metal base to cause.The casting porcelain makes neck portion also can reach good aesthetic then with the good transparency and refractivity and high-intensity interior being preced with solved this beauty treatment chronic disease.
2, gum is healthy: the nickel chromium triangle metal is claimed base metal again, and gum is had more serious stimulation, and groups of people, especially women to its allergy, cause gum swelling, hemorrhage, even has the patient also irritated to precious metal; The casting porcelain is not then found responsive case basically.
3, gingival discoloration: base metal oxidation in the oral cavity forms the grey oxide compound, is dispersed in and deposits to gingival edge, causes that reason becomes ash, influences attractive in appearance; The casting porcelain this problem can not occur.
4, inside and outside hat combines: the combination of metal and porcelain is a weak ring, often can see porcelain and metal-stripping, exposes the situation of greyish black metal.The casting porcelain is because inside and outside hat all is a porcelain, and the combination of porcelain and porcelain is best certainly.
5, the hardness of ceramic crown can cause the wearing and tearing to the jaw tooth greater than enamel.And the hardness of IPS Empress casting porcelain is similar to enamel, and the jaw tooth is worn and torn synchronously.
6, there is not metal to disturb, to possible from now on not influence of CT nuclear-magnetism inspection.
7, under special occasions light, do not have unusual blueness.
The casting porcelain of using in the market exists the price height, and energy consumption is big, high heat colouring difficulty, and complex forming technology, product size is single, and appointed condition requires high shortcoming.And casting the main preparation method of porcelain at present is main with high-temperature melting method, and this method power consumption is big, and high heat colouring conditional request is high, complex forming technology.
Both at home and abroad the researchist to two lithium silicates as the sytull of principal crystalline phase as one of research emphasis; Wherein, USP discloses the technology of preparing and the material property of this kind material, but the preparation method is a high-temperature melting method, does not relate to the sintering process preparation.In the domestic patent; Like the patent No. is that ZL200810226527.0, CN200710072597.0, CN200510010431.7, CN200910043711.6 etc. have mentioned this kind preparation methods; Also adopted the sintering process preparation; But all be once painted, do not mention the process method of secondary coloring, and intensity does not all surpass 350MPa.And appointed condition requires high, complicated process of preparation.
Summary of the invention
The present invention be directed to the problem that prior art exists, provide a kind of energy consumption low, painted simple to operation, moulding process is simple, product size variation, good repetitiveness, constant product quality, the preparation method of a kind of lithium base casting porcelain porcelain piece that intensity is high.
The present invention is formulated by ratio of weight and the number of copies by following base starting material:
Silicon-dioxide (SiO 2): 65-75;
Aluminum oxide (Al 2O 3): 1-5;
Lithium Oxide 98min (Li 2O): 13-16;
Potassium oxide (K 2O): 2-5;
Vanadium Pentoxide in FLAKES (P 2O 5): 2-5;
Zirconium white (ZrO 2): 1-5;
Boron oxide (B 2O 3): 2-5
Silicon-dioxide (SiO wherein 2) and Lithium Oxide 98min (Li 2O) mol ratio is SiO 2: Li 2O=2.30-2.50: 1;
Its preparation method comprises the steps:
First step: get various base starting materials by the described ratio of weight and number of claim 1, mixed in 2 hours through ball mill grinding;
Second step: above-mentioned mixed raw material powder is packed in the platinum crucible, heat, when making temperature rise to 1500 ℃, be incubated 1 hour, make the raw material fusing, obtain uniform glass metal;
Third step: with second step is that the glass metal that obtains carries out shrend, obtains tiny glass block, places 120 ℃ of oven dry down;
The 4th step: the glass block that third step is obtained is put into agate jar and is carried out ball mill pulverizing, and the powder of adding and agate ball material ball ratio by weight are that the ratio of 1:2 was ground 40 hours, obtain glass powder, cross 300 mesh sieves, obtain glass powder;
The 5th step: the glass powder that the 4th step is obtained by ratio of weight and the number of copies, the ratio of glass powder: tinting material=10:1-20:1 and tinting material mixing 1-3 hour mix it, obtain mixed powder;
The 6th step: the mixed powder that the 5th step is obtained is packed in the mould, isostatic pressing, and pressure is 150-250MPa, obtains casting the porcelain base substrate;
The 7th step: the casting porcelain base substrate that the 6th step obtains is put into the resistance furnace sintering, and temperature rise rate is 10 ℃/minute, is warming up to sintering temperature 880-920 ℃, and soaking time is 10-60 minute, and furnace cooling promptly gets and casts porcelain porcelain piece.
Advantageous effect of the present invention is following:
The present invention adopts sintering process to prepare the dentistry microcrystal glass material, and adopts secondary coloring technology to carry out painted.Only need disposable preparation host glass powder, need not cleaning crucible; Do not worry the aberration that variable valency metal ions high temperature appraises at the current rate and brings, and can produce the different colours product, uniform coloring, color is pure; Moulding is easy to operate, and product size can realize variation; It is low to produce power consumption, save energy, thus practiced thrift production cost, thus energy problem solved.With the product of this method preparation, the high energy of its intensity reaches 380MPa, and density reaches 2.478g/cm 3
Product of the present invention also has excellent biological compatibility, creamy white, shape and Stability Analysis of Structures; Advantages such as preparation technology is simple, production cost is low; Also can not need any processing just can use after the processing through being machined into the very accurate and various goods of pattern of size.Substituted metal porcelain tooth just progressively is widely used in the dental prosthetic field at present.Because therefore raw materials used being easy to get of production product of the present invention be very suitable for industrialization, has the development and application prospect.
Embodiment
The substrate material of a kind of lithium base casting porcelain porcelain piece of the present invention is formulated by ratio of weight and the number of copies by following base starting material:
Silicon-dioxide (SiO 2) : 68.5;
Aluminum oxide (Al 2O 3) : 3;
Lithium Oxide 98min (Li 2O): 14.5;
Potassium oxide (K 2O): 4;
Vanadium Pentoxide in FLAKES (P 2O 5): 3;
Zirconium white (ZrO 2): 3;
Boron oxide (B 2O 3): 4;
Silicon-dioxide (SiO wherein 2) and Lithium Oxide 98min (Li 2O) mol ratio is SiO 2: Li 2O=2.35:1.
The preparation of host glass powder:
First step: get various base starting material 200g, wherein SiO by above-mentioned ratio of weight and number 2107.4g; Al (OH) 35.5g; Li 2CO 356.2g; K 2CO 39.2g; Al (PO 3) 35.9g; ZrO 24.7g; H 3BO 311.1g, mixed in 2 hours through ball mill grinding;
Second step: above-mentioned mixed raw material powder is packed in the platinum crucible, heat up, when making temperature rise to 1500 ℃, be incubated 1 hour raw material is melted, obtain uniform glass metal;
Third step: the glass metal that second step is obtained carries out shrend, obtains tiny glass block, places 120 ℃ of oven dry down;
The 4th step: the glass block that third step is obtained is put into agate jar, add agate ball, and expect by weight: the ratio of ball=1:2 is carried out ball mill pulverizing, grinds 40 hours, obtains glass powder, crosses 300 mesh sieves, and it is subsequent use to obtain glass powder.
Embodiment 1
First step: the above-mentioned glass powder of obtaining is got 50g, and weighing tinting material red stone 5g, the ratio of glass powder: red stone=10:1 is put into ball grinder mixing 3 hours by weight, and it is mixed, and obtains mixed powder;
Second step: the mixed powder that first step is obtained is packed in the mould, isostatic pressing, and pressure is 250MPa, obtains casting the porcelain base substrate;
Third step: the casting porcelain base substrate that second step obtains is put into the resistance furnace sintering, and temperature rise rate is 10 ℃/minute, 920 ℃ of intensification sintering temperatures; Soaking time is 10 minutes; Furnace cooling promptly obtains casting ceramic material, lithium abutment promptly of the present invention section casting porcelain porcelain piece.
Embodiment 2
First step: the host glass powder of above-mentioned gained is got 50g, and weighing tinting material red stone 2.5g, the ratio of glass powder: red stone=20:1 is put into ball grinder mixing 2 hours by weight, and it is mixed, and obtains mixed powder;
Second step: above-mentioned mixed powder is packed in the mould, isostatic pressing, pressure is 200MPa, obtains casting the porcelain base substrate;
Third step: with second step is that the casting porcelain base substrate that obtains is put into the resistance furnace sintering, and temperature rise rate is 10 ℃/minute, 900 ℃ of intensification sintering temperatures; Soaking time is 30 minutes; Furnace cooling promptly obtains casting ceramic material, lithium abutment promptly of the present invention section casting porcelain porcelain piece.
Embodiment 3
First step: the host glass powder of above-mentioned gained is got 50g, and weighing tinting material red stone 3.3g, the ratio of glass powder: red stone=15:1 is put into ball grinder mixing 1 hour by weight, and it is mixed, and obtains mixed powder;
Second step: above-mentioned mixed powder is packed in the mould, isostatic pressing, pressure is 150MPa, obtains casting the porcelain base substrate;
Third step: with second step is that the casting porcelain base substrate that obtains is put into the resistance furnace sintering, and temperature rise rate is 10 ℃/minute, 880 ℃ of intensification sintering temperatures; Soaking time is 60 minutes; Furnace cooling promptly obtains casting ceramic material, lithium abutment promptly of the present invention section casting porcelain porcelain piece.
Embodiment 4
The present invention is formulated by ratio of weight and the number of copies by following base starting material:
Silicon-dioxide (SiO 2): 65;
Aluminum oxide (Al 2O 3): 1;
Lithium Oxide 98min (Li 2O): 13;
Potassium oxide (K 2O): 2;
Vanadium Pentoxide in FLAKES (P 2O 5): 2;
Zirconium white (ZrO 2): 1;
Boron oxide (B 2O 3): 2; Its preparation technology is with embodiment 1.
Embodiment 5
The present invention is formulated by ratio of weight and the number of copies by following base starting material:
Silicon-dioxide (SiO 2): 75;
Aluminum oxide (Al 2O 3): 5;
Lithium Oxide 98min (Li 2O): 16;
Potassium oxide (K 2O): 5;
Vanadium Pentoxide in FLAKES (P 2O 5): 5;
Zirconium white (ZrO 2): 5;
Boron oxide (B 2O 3): 5; Its preparation technology is with embodiment 1.

Claims (3)

1. the preparation method of lithium base casting porcelain porcelain piece is characterized in that by following base starting material formulated by ratio of weight and the number of copies:
Silicon-dioxide (SiO 2): 65-75;
Aluminum oxide (Al 2O 3): 1-5;
Lithium Oxide 98min (Li 2O): 13-16;
Potassium oxide (K 2O): 2-5;
Vanadium Pentoxide in FLAKES (P 2O 5): 2-5;
Zirconium white (ZrO 2): 1-5;
Boron oxide (B 2O 3): 2-5
Silicon-dioxide (SiO wherein 2) and Lithium Oxide 98min (Li 2O) mol ratio is SiO 2: Li 2O=2.30-2.50: 1;
Its preparation method comprises the steps:
First step: get various base starting materials by the described ratio of weight and number of claim 1, mixed in 2 hours through ball mill grinding;
Second step: above-mentioned mixed raw material powder is packed in the platinum crucible, heat, when making temperature rise to 1500 ℃, be incubated 1 hour, make the raw material fusing, obtain uniform glass metal;
Third step: the glass metal that second step is obtained carries out shrend, obtains tiny glass block, places 120 ℃ of oven dry down;
The 4th step: the glass block that third step is obtained is put into agate jar and is carried out ball mill pulverizing, and the powder of adding and agate ball material ball ratio by weight are that the ratio of 1:2 was ground 40 hours, obtain glass powder, cross 300 mesh sieves, obtain glass powder;
The 5th step: the glass powder that the 4th step is obtained by ratio of weight and the number of copies, the ratio of glass powder: tinting material=10:1-20:1 and tinting material mixing 1-3 hour mix it, obtain mixed powder;
The 6th step: the mixed powder that the 5th step is obtained is packed in the mould, isostatic pressing, and pressure is 150-250MPa, obtains casting the porcelain base substrate;
The 7th step: the casting porcelain base substrate that the 6th step obtains is put into the resistance furnace sintering, and temperature rise rate is 10 ℃/minute, is warming up to sintering temperature 880-920 ℃, and soaking time is 10-60 minute, and furnace cooling promptly gets and casts porcelain porcelain piece.
2. the preparation method of lithium base casting porcelain porcelain piece according to claim 1 is characterized in that described base starting material is formulated by following ratio of weight and number:
Silicon-dioxide (SiO 2): 68.5;
Aluminum oxide (Al 2O 3): 3;
Lithium Oxide 98min (Li 2O): 14.5;
Potassium oxide (K 2O): 4;
Vanadium Pentoxide in FLAKES (P 2O 5): 3;
Zirconium white (ZrO 2): 3;
Boron oxide (B 2O 3): 4;
In described the 5th step, by ratio of weight and the number of copies, the ratio of glass powder: tinting material=10:1 is put into ball grinder and was mixed 3 hours;
The described the 6th rapid in, pressure is 250MPa;
In described the 7th step, temperature rise rate is 10 ℃/minute, and 920 ℃ of intensification sintering temperatures, soaking time are 10 minutes.
3. the preparation method of lithium base casting porcelain porcelain piece according to claim 1 and 2 is characterized in that described tinting material is a red stone.
CN2010106042724A 2010-12-24 2010-12-24 Novel method for preparing lithium-based casting ceramic block Active CN102153284B (en)

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Publication number Priority date Publication date Assignee Title
CN102976617B (en) * 2012-11-30 2015-04-15 华泽庆 Glass ceramic and preparation method thereof
EP2995434B1 (en) 2013-05-10 2020-02-19 Kuraray Noritake Dental Inc. Methods for producing zirconia sintered bodies, zirconia compositions and zirconia calcined bodies
CN107265867B (en) * 2017-06-16 2020-09-04 有研医疗器械(北京)有限公司 Lithium-based glass ceramic powder for dental restoration and preparation method thereof
CN114409430B (en) * 2022-01-04 2022-11-04 北京劲松口腔医院投资管理有限公司 All-ceramic prosthesis and preparation process thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6802894B2 (en) * 1998-12-11 2004-10-12 Jeneric/Pentron Incorporated Lithium disilicate glass-ceramics
US7452836B2 (en) * 2005-02-08 2008-11-18 Ivoclar Vivadent Ag Lithium silicate glass ceramic

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6802894B2 (en) * 1998-12-11 2004-10-12 Jeneric/Pentron Incorporated Lithium disilicate glass-ceramics
US7452836B2 (en) * 2005-02-08 2008-11-18 Ivoclar Vivadent Ag Lithium silicate glass ceramic

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Title
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金迎辉等.稀土La2O3对Li2O-Al2O3-SiO2微晶玻璃结构和性能的影响.《佛山陶瓷》.2002,(第7期), *

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