CN104990412A - Microwave hot isostatic pressure sintering furnace for dental zirconia ceramic later sintering - Google Patents
Microwave hot isostatic pressure sintering furnace for dental zirconia ceramic later sintering Download PDFInfo
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- CN104990412A CN104990412A CN201510485341.7A CN201510485341A CN104990412A CN 104990412 A CN104990412 A CN 104990412A CN 201510485341 A CN201510485341 A CN 201510485341A CN 104990412 A CN104990412 A CN 104990412A
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Abstract
The invention provides a microwave hot isostatic pressure sintering furnace for dental zirconia ceramic later sintering. The microwave hot isostatic pressure sintering furnace comprises an upper cover, a plug and a furnace body. A high-pressure cylinder body made of silicon carbide is arranged at the upper portion of the furnace body. The high-pressure cylinder body is wrapped by a lower insulating layer. An anti-explosion layer is arranged on the outer side of the lower insulating layer. A cooling layer is arranged on the outer side of the anti-explosion layer. A furnace outer shell is arranged on the outer side of the cooling layer. A microwave generator is arranged at the lower portion of the furnace body. The plug is a T-shaped plug. A body of the plug is made of silicon carbide, the plug cap portion of the body is wrapped by an upper insulating layer, and a high-pressure gas pipe and an optical pyrometer are arranged in the middle of the plug. The top face of the inner side of a cover body of the upper cover is connected with a disc-shaped pressure buckle. The microwave hot isostatic pressure sintering furnace can well improve bending strength and breaking tenacity of dental ceramic and improve safety of the dental ceramic. Materials used for the sintering furnace are simple, price is low, maintenance cost is low, mass production is easy, and the sintering furnace can be popularized to county-level professional dental departments.
Description
Technical field
The present invention relates to a kind of agglomerating plant of dental zirconium oxide pottery, specifically a kind of microwave thermal isostatic sintering stove for dental zirconium oxide pottery later stage sintering.
Background technology
Zirconium oxide full-porcelain has firm wear-resisting, the multiple advantage such as appearance color and luster is true to nature, good biocompatibility, and not containing metal, non-stimulated to gum, gum can not be caused to turn green phenomenon, can not be irritated, so Zirconium oxide full-porcelain reparation is the fashion trend that international dental prosthetics is repaired, it is also the focus in current international dentistry market.
The technological process of current Dental firing zirconia ceramics is first after zirconia powder and the abundant banburying of additive, block or rod is compacted into through isostatic cool pressing 100MPa, then thermal debinding is added, pre-burning to 900 ~ 1000 DEG C, use computer CAD/CAM automation equipment fine finishining biscuit again, finally become ceramic product by concora crush high temperature sintering 1500 DEG C again.
The sintering process of dental zirconium oxide pottery mainly contains concora crush sintering, hot pressed sintering, gas pressure sintering, HIP sintering, discharge plasma sintering and microwave sintering etc., wherein HIP sintering effect is best, can also the product of sintered shape complexity, but HIP sintering apparatus expensive, operation and maintenance expense is all very high.And concora crush sintering is the most simply saved trouble, equipment is also inexpensive, but its brittleness of ceramics sintered out is large.
Domestic current dental zirconium oxide pottery concora crush sintering technology has Ai Er to create patent of invention (CN102028624B) product of company preferably, and its bending strength is 450 ~ 550Mpa, and fracture toughness is 9 ~ 10Mpam
1/2.And opaque ceramic tooth stake patent of invention (CN1489987A) product that Tsing-Hua University and BJ Stomatological Hospital develop, its bending strength is 600Mpa, and fracture toughness is 13Mpam
1/2.These products be used as corona and tooth stake performance still can, the thinner planting body of labial teeth or the full porcelain planting body of two-part be done, poor reliability, during fracture, want to take out all difficulties.
Concora crush sintering in atmosphere, as CeO in zirconia
2when content is 12%, the product bending strength sintered out is 700 ~ 800Mpa, and fracture toughness is 9.5 ~ 10Mpam
1/2.According to made, the people such as foreign study personnel Tsukuma are with cerium zirconia product 12Ce-TZP biscuit after 1400 DEG C of concora crush sintering, then in temperature 1500 DEG C, HIP sintering 2 hours under air pressure 200Mpa, the fracture toughness of its product can reach 30Mpam
1/2, and there is not mechanics degradation phenomena.And with yttrium zirconia product 3Y-TZP biscuit temperature 1500 DEG C, air pressure 200Mpa, HIP sintering 2 hours, the fracture toughness of its product can reach 18Mpam
1/2.
According to another Tsing-Hua University professor Xie Zhipeng to the research of high strength oxide ceramics, oxide ceramics carries out high temperature insostatic pressing (HIP) (HIP) process in oxidizing atmosphere, performance is better than hip treatment in inert atmosphere, hip treatment equally, oxidizing atmosphere process makes the bending strength of yttrium zirconia product Y-PSZ bring up to 1500Mpa or higher by 1000Mpa, and sintering can make cerium zirconia products C e-TZP color be shoaled by the black look that exhausts in oxidizing atmosphere, be applicable to doing tooth implant, the light transmittance of yttrium zirconia product Y-TZP can be made to increase, be applicable to doing corona, attractive in appearance.
Summary of the invention
The object of this invention is to provide a kind of microwave thermal isostatic sintering stove for dental zirconium oxide pottery later stage sintering, with this sintering furnace, later-stage secondary sintering is carried out to the dental zirconium oxide pottery that concora crush sinters out, both significantly can save the production cost of product, properties of product can be made again to meet the demand of dental applications.
Concrete technical scheme of the present invention is as follows:
For a microwave thermal isostatic sintering stove for dental zirconium oxide pottery later stage sintering, it is characterized in that: comprise upper cover, stopper and body of heater, wherein stopper fills in the top of body of heater, and upper cover is formed from top fastening body of heater and to stopper and pushes up pressure;
The top of described body of heater is provided with the high pressure cylinder body that a carborundum is made, the cylinder holes at high pressure cylinder body end face center is a two stage steps hole, wherein going up hole, rank is obturating plug hole, hole, lower rank is burner hearth, the outside of high pressure cylinder body is enclosed with the lower thermal insulation layer be wound with quartz fibre, the outside of lower thermal insulation layer is also provided with the explosion-proof layer formed with steel wire winding, the outside of explosion-proof layer is provided with the cooling layer be built into water-cooled copper, it is body of heater shell outside cooling layer, the bottom of body of heater is provided with a microwave generator, microwave generator is positioned at the below of high pressure cylinder body, its emitting head faces the burner hearth of high pressure cylinder body, bottom high pressure cylinder body explosion-proof layer, the position of corresponding microwave generator emitting head has the bottom outlet passed through for microwave, body of heater shell upper edge is provided with external screw teeth or draw-in groove,
Described stopper is a T-shaped plug, its main body adopts carborundum to make, the outside of the cock cap part of main body is enclosed with the upper thermal insulation layer be wound with quartz fibre, corresponding with the lower thermal insulation layer of body of heater, and the middle part of stopper is provided with runs through upper and lower high-pressure air pipe and leucoscope;
Inside the lid of described upper cover, end face is connected with a dish type pressure by screw rod and kowtows, screw rod is also set with stage clip, lid end face and pressure are kowtowed end face and are all had the through hole supplying the high-pressure air pipe of stopper to stretch out, and upper cap body lower edges is provided with the internal screw thread suitable with body of heater shell or fixture block.
In order to realize better sealing, the external cylindrical surface of the cock body part of described plug body and step surface are enclosed with one deck sealing pyrophillite.
In order to prevent microwave from leakage, described body of heater shell and upper cap body adopt stainless steel material to make.
Microwave thermal isostatic sintering stove of the present invention adopts microwave and hot oxygen to press the mode of conbined usage to carry out later-stage secondary sintering to the dental zirconium oxide pottery that concora crush sinters out, HTHP sintering effectively can eliminate the residual porosity of concora crush sintered products, increase its density, and eliminate its internal stress, bending strength and the fracture toughness of dental polishing can be improved well, make properties of product meet the demand of dental applications.Because microwave sintering is by microwave electromagnetic field and material medium interaction self-heating, there is no external heat source, so intensification block, homogeneous heating.Zirconia is at room temperature very little to microwave absorption, just strong absorption is had to microwave after being only heated to above critical point temperature, and carborundum at room temperature just absorbs microwave generation heating, and carborundum is high temperature resistant, therefore the high pressure cylinder body made with carborundum and stopper build burner hearth, can effectively preheat the dental zirconium oxide pottery in burner hearth, until its temperature is higher than critical point and own absorption microwave heating.Quartz fibre has good permeability to microwave in addition, and without heating, employing quartz fibre both can be heat insulation as the thermal insulation layer of body of heater, and the explosion-proof layer associating that can be formed with steel wire winding is again explosion-proof.The cooling layer that water-cooled copper builds mainly plays the effect of radiating and cooling.This microwave thermal isostatic sintering stove uses material simple, and cheap, maintenance cost is few, easy mass production, can spread to county's one-level dental professional.
Accompanying drawing explanation
Fig. 1 is the overall structure schematic diagram of microwave thermal isostatic sintering stove of the present invention.
Fig. 2 is the structural representation of upper cover.
Fig. 3 is the structural representation of stopper.
Fig. 4 is the structural representation of body of heater.
In figure: 1-upper cover, 2-stopper, 3-body of heater, 4-dental zirconium oxide pottery, 5-quartz fiber cloth, 6-through hole, 7-screw rod, 8-stage clip, 9-pressure is kowtowed, 10-lid, 11-internal screw thread, 12-high-pressure air pipe, 13-leucoscope, 14-plug body, the upper thermal insulation layer of 15-, 16-seals pyrophillite, 17-burner hearth, 18 obturating plug holes, 19-high pressure cylinder body, thermal insulation layer under 20-, 21-explosion-proof layer, 22-external screw teeth, 23-cooling layer, 24-bottom outlet, 25-microwave emitter, 26-body of heater shell, 27-Microwave emission head.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention will be further described.
As shown in Figure 1, microwave thermal isostatic sintering stove of the present invention comprises upper cover 1, stopper 2 and body of heater 3, and wherein stopper 2 fills in the top of body of heater 3, and upper cover 1 is formed from top fastening body of heater 3 and to stopper 2 and pushes up pressure.
As shown in Figure 4, the top of described body of heater 3 is provided with the high pressure cylinder body 19 that a carborundum is made, the cylinder holes at high pressure cylinder body 19 end face center is a two stage steps hole, wherein going up hole, rank is obturating plug hole 18, hole, lower rank is burner hearth 17, the outside of high pressure cylinder body 19 is enclosed with the lower thermal insulation layer 20 be wound with quartz fibre, the outside of lower thermal insulation layer 20 is also provided with the explosion-proof layer 21 formed with steel wire winding, the outside of explosion-proof layer 21 is provided with the cooling layer 23 be built into water-cooled copper, it is body of heater shell 26 outside cooling layer 23, the bottom of body of heater 3 is provided with a microwave generator 25, microwave generator 25 is positioned at the below of high pressure cylinder body 19, its emitting head 27 faces the burner hearth 17 of high pressure cylinder body 19, bottom high pressure cylinder body explosion-proof layer 21, the position of corresponding microwave generator emitting head 27 has the bottom outlet 24 passed through for microwave, body of heater shell 26 upper edge is along being provided with external screw teeth 22.
As shown in Figure 3, described stopper 2 is a T-shaped plug, its main body 14 adopts carborundum to make, the outside of the cock cap part of main body 14 is enclosed with the upper thermal insulation layer 15 be wound with quartz fibre, corresponding with the lower thermal insulation layer 20 of body of heater 3, the external cylindrical surface of the cock body part of main body 14 and step surface are enclosed with one deck sealing pyrophillite 16, and the middle part of stopper 2 is provided with the high-pressure air pipe 12 and leucoscope 13 that run through upper and lower.
As shown in Figure 2, inside the lid 10 of described upper cover 1, end face is connected with a dish type pressure by screw rod 7 and kowtows 9, screw rod 7 is also set with stage clip 8, lid 10 end face and pressure are kowtowed 9 end faces and are all had the through hole 6 supplying the high-pressure air pipe 12 of stopper 2 to stretch out, and upper cap body 10 lower edges is provided with the internal screw thread 11 suitable with body of heater shell 26.
Applying dental zirconium oxide pottery that microwave thermal isostatic sintering stove of the present invention sinters out to concora crush, to carry out the step of later-stage secondary sintering as follows:
1), the upper cover 1 of this sintering furnace and stopper 2 are taken apart from body of heater 3, the dental zirconium oxide pottery 4 sintering out by concora crush is wrapped by quartz fiber cloth 5 and is put into the burner hearth 17 of body of heater 3, then stopper 2 is filled in body of heater 3, and upper cover 1 is tightened above body of heater 3, the end face making the pressure of upper cover 1 kowtow 9 pairs of stoppers 2 forms top pressure.
Dental zirconium oxide pottery 4 outsourcing quartz fiber cloth 5 occur thermal runaway in order to contact zone temperature anomaly when preventing heating using microwave raises, by parcel quartz fiber cloth 5, when silicon carbide hearth 17 can be avoided directly to contact with dental zirconium oxide pottery 4, contact zone heat transfer is too fast, and the contradiction that dental zirconium oxide pottery 4 therein heat transfer are excessively slow.
2), from outside by the introducing high-pressure air pipe 12 of high pressure oxygen-containing gas, by the controller of this sintering furnace, the pressure introducing high pressure oxygen-containing gas is controlled, the feedback line of leucoscope 13 is also connected with Time Controller, and control the heating work of microwave generator 25, thus realize heating-up temperature and the control of heat time.
3) the dental zirconium oxide pottery 4, started in microwave generator 25 pairs of burner hearths 17 by controller is heated, with high pressure oxygen-containing gas, under oxidizing atmosphere, isostatic pressed pressurization is carried out to it simultaneously, slow intensification 3 hours, temperature rises to 1500 DEG C, air pressure rises to 200MPa, maintain HTHP 2 hours, and then slow cooling step-down 2 is little of normal temperature and pressure.
In described step 2, the gases at high pressure of introducing can be the mixture of oxygen or nitrogen and oxygen.
In addition, for the dental zirconium oxide pottery 4 preferably enhancement mode compound zirconia ceramic material of double sintering, wherein cerium zirconia ceramics increase toughness is maximum, and without mechanics degradation phenomena, its its colour changed into yellow, is applicable to doing tooth implant; And yttrium zirconia ceramics is gained in strength maximum, its transparency increases, attractive in appearance, is applicable to doing corona.
Claims (6)
1. the microwave thermal isostatic sintering stove for dental zirconium oxide pottery later stage sintering, it is characterized in that: comprise upper cover (1), stopper (2) and body of heater (3), wherein stopper (2) fills in the top of body of heater (3), and upper cover (1) is formed from top fastening body of heater (3) and to stopper (2) and pushes up pressure;
The top of described body of heater (3) is provided with the high pressure cylinder body (19) that a carborundum is made, the cylinder holes at high pressure cylinder body (19) end face center is a two stage steps hole, wherein going up hole, rank is obturating plug hole (18), hole, lower rank is burner hearth (17), the outside of high pressure cylinder body (19) is enclosed with the lower thermal insulation layer (20) be wound with quartz fibre, the outside of lower thermal insulation layer (20) is also provided with the explosion-proof layer (21) formed with steel wire winding, the outside of explosion-proof layer (21) is provided with the cooling layer (23) be built into water-cooled copper, cooling layer (23) outside is body of heater shell (26), the bottom of body of heater (3) is provided with a microwave generator (25), microwave generator (25) is positioned at the below of high pressure cylinder body (19), its emitting head (27) faces the burner hearth (17) of high pressure cylinder body (19), the position of the corresponding microwave generator emitting head (27) in high pressure cylinder body explosion-proof layer (21) bottom has the bottom outlet (24) passed through for microwave, body of heater shell (26) upper edge is along being provided with external screw teeth (22) or draw-in groove,
Described stopper (2) is a T-shaped plug, its main body (14) adopts carborundum to make, the outside of the cock cap part of main body (14) is enclosed with the upper thermal insulation layer (15) be wound with quartz fibre, corresponding with the lower thermal insulation layer (20) of body of heater (3), the middle part of stopper (2) is provided with the high-pressure air pipe (12) and leucoscope (13) that run through upper and lower;
Lid (10) the inner side end face of described upper cover (1) is connected with a dish type pressure by screw rod (7) and kowtows (9), screw rod (7) is also set with stage clip (8), lid (10) end face and pressure are kowtowed (9) end face and are all had the through hole supplying the high-pressure air pipe (12) of stopper (2) to stretch out, and upper cap body (10) lower edges is provided with the internal screw thread (10) suitable with body of heater shell (26) or fixture block.
2. sintering furnace according to claim 1, is characterized in that: the external cylindrical surface of the cock body part of described plug body (14) and step surface are enclosed with one deck sealing pyrophillite (16).
3. sintering furnace according to claim 1, is characterized in that: described body of heater shell (26) and upper cap body (10) adopt stainless steel material to make.
4. apply sintering furnace as claimed in claim 1 carries out a later-stage secondary sintering method to the dental zirconium oxide pottery that concora crush sinters out, comprise the steps:
1), the upper cover (1) of this sintering furnace and stopper (2) are taken apart from body of heater (3), (4 to wrap by quartz fiber cloth (5) and to put into the burner hearth (17) of body of heater (3) for the dental zirconium oxide pottery that sinters out by concora crush, then stopper (2) is filled in body of heater (3), and upper cover (1) is tightened in body of heater (3) top, make the pressure of upper cover (1) kowtow (9) and top pressure is formed to the end face of stopper (2);
2), from outside by the introducing high-pressure air pipe (12) of high pressure oxygen-containing gas, by the controller of this sintering furnace, the pressure introducing high pressure oxygen-containing gas is controlled, the feedback line of leucoscope (13) is also connected with Time Controller, and control the heating work of microwave generator (25), thus realize heating-up temperature and the control of heat time;
3), start microwave generator (25) by controller to heat the dental zirconium oxide pottery (4) in burner hearth (17), under oxidizing atmosphere, isostatic pressed pressurization is carried out to it with high pressure oxygen-containing gas simultaneously, slow intensification 3 hours, temperature rises to 1500 DEG C, air pressure rises to 200MPa, maintain HTHP 2 hours, and then slow cooling step-down 2 is little of normal temperature and pressure.
5. method according to claim 4, is characterized in that: in described step 2, and the gases at high pressure of introducing are the mixture of oxygen or nitrogen and oxygen.
6. method according to claim 4, is characterized in that: the dental zirconium oxide pottery 4 for double sintering adopts enhancement mode compound zirconia ceramic material, wherein adopts cerium zirconia ceramics to do tooth implant, adopts yttrium zirconia ceramics to do corona.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN201510485341.7A CN104990412B (en) | 2015-08-10 | 2015-08-10 | Microwave hot isostatic pressure sintering furnace for dental zirconia ceramic later sintering |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110891921A (en) * | 2017-07-31 | 2020-03-17 | 可乐丽则武齿科株式会社 | Zirconia sintered body containing fluorescent agent |
| CN115321960A (en) * | 2022-08-22 | 2022-11-11 | 南充三环电子有限公司 | Alumina ceramic and preparation method and application thereof |
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2015
- 2015-08-10 CN CN201510485341.7A patent/CN104990412B/en not_active Expired - Fee Related
Patent Citations (8)
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| DE3630049A1 (en) * | 1986-09-04 | 1988-03-24 | Schott Verwaltung | Method and device for melting wax models or wax model clusters out of ceramic investment casting moulds |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110891921A (en) * | 2017-07-31 | 2020-03-17 | 可乐丽则武齿科株式会社 | Zirconia sintered body containing fluorescent agent |
| CN115321960A (en) * | 2022-08-22 | 2022-11-11 | 南充三环电子有限公司 | Alumina ceramic and preparation method and application thereof |
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| CN104990412B (en) | 2017-03-22 |
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