CN101765255A - Immersion type hot-dip plating composite ceramic protecting pipe and preparation method thereof - Google Patents

Immersion type hot-dip plating composite ceramic protecting pipe and preparation method thereof Download PDF

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CN101765255A
CN101765255A CN201010104190A CN201010104190A CN101765255A CN 101765255 A CN101765255 A CN 101765255A CN 201010104190 A CN201010104190 A CN 201010104190A CN 201010104190 A CN201010104190 A CN 201010104190A CN 101765255 A CN101765255 A CN 101765255A
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pipe
ceramic
composite
outer tube
sic
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CN101765255B (en
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金志浩
杨万利
李红伟
乔冠军
金海云
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Xian Jiaotong University
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Xian Jiaotong University
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Abstract

The invention discloses an immersion type hot-dip plating composite ceramic protecting pipe and a preparation method thereof; an outer pipe green body with one end closed is prepared by composite SiC ceramic material; a composite Si3N4 coating layer is coated on the outer pipe green body, and the coating layer and the outer pipe green body are sintered to obtain the composite SiC ceramic outer pipe under the nitrogen protection; and then an inner pipe green body with one end closed is prepared by SiC or AlN base ceramic material, and reaction and sintering are carried out to obtain the SiC or AlN base ceramic inner pipe; low-melting-point ceramic glaze is coated in the outer pipe or outside the inner pipe, the inner pipe is assembled in the outer pipe to carry out heat treatment, and the inner pipe is firmly bonded in the outer pipe to obtain the ceramic protecting pipe. By compositing the inner and outer different ceramic materials, the requirements of comprehensive performances such as no immersion, no leakage, no corrosion, high thermal shock resisting force, no crack caused by chilling and heat shock, good heat conduction and the like of the protecting pipe and the molten liquid are met, and the protecting pipe has the advantages of high intensity and long service life.

Description

Immersion type hot-dip plating composite ceramic protecting pipe and preparation method
Technical field
The present invention relates to structure of a kind of immersion type hot-dip plating composite ceramic protecting pipe and preparation method thereof.
Background technology
In hot-dip (Zn, Al) industry, die casting (Al, Zn, Mg etc.) industry, its hot-dip coating installation and die casting machine fusing of margin holding furnace mainly adopt external-heat, adopt coal, oil, gas etc. to do thermal source and iron and steel crucible molten bath.The subject matter of firing equipment is that (1) heat efficiency is low, generally only 20~30%, and energy consumption is big, and environmental pollution is big.(2) because high-temperature metal liquid (Al, Zn, Mg etc.) and iron and steel crucible generation chemical reaction generate slag and ashes, crucible life short (several months) not only, also a large amount of loss feed metals (Al, Zn, Mg).(3) because the temperature control difficulty is big, the slag ashes are many, cause product quality problem.In order to overcome above-mentioned shortcoming, people adopt ceramic crucible, and immersion (internal heat type) method that adopts heating element with ceramic protecting pipe to come metal in the heating ceramic crucible, and its heat efficiency can reach more than 70~80%, and the ceramic crucible life-span can reach 10 years.Its core technology is the ceramic protecting pipe of heating element.Its claimed tube material and metal liquid (Al, Zn Mg) do not soak into, do not leak, do not corrode, thermal shock drag height, and chilling and shock heating does not ftracture, and thermal conductance is good, the intensity height, the life-span is long.
Find heated protective pipe in homogenous material metal or the ceramic making by the experimental study of many decades both at home and abroad.As the difficult erosion of infusibility metal, SiC, Si 3N 4, Sialon, Al 2O 3, ZrO 2Etc. advanced structural ceramic commonly used, all be difficult to satisfy above-mentioned combination property.
Summary of the invention
Adopt the existing problem of heated protective pipe in single metal or the ceramic making for solving, the invention provides a kind of composite ceramic protection tube and preparation method,
For reaching above purpose, the present invention takes following technical scheme to be achieved:
A kind of immersion type hot-dip plating composite ceramic protecting pipe comprises the composite SiC pottery outer tube that an end seals, and this outer tube outer wall is provided with composite S i 3N 4Coat is provided with pipe in SiC or the AlN base pottery in this outer tube, described interior Guan Yiduan is used to install the heater element that stretches into wherein; The other end external shape of interior pipe just matches with the interior shape of outer duct occlusion one end; Be low melting point ceramic glaze bonding transition zone between described outer tube and interior pipe.
The preparation method of aforementioned immersion type hot-dip plating composite ceramic protecting pipe comprises the steps
(1) prepares the outer tube biscuit that an end seals with the composite SiC ceramic material with the isostatic compaction method;
(2) coating composite S i on the outer tube biscuit 3N 4Coat, coat gets composite SiC pottery outer tube with outer tube biscuit 1450~1600 ℃ of sintering under nitrogen protection;
(3) prepare the interior pipe biscuit of end sealing with extruding or isostatic compaction method with SiC or AlN base ceramic material, 1450~1600 ℃ of reaction-sintereds get pipe in SiC or the AlN base pottery, and the external shape of Guan Yiduan just matches with the interior shape of outer duct occlusion one end of pottery in this pottery;
(4) the low melting point ceramic glaze is coated in step (2) the gained composite SiC pottery outer tube or step (3) gained in outside the pipe, fit into interior pipe in the outer tube after, in 700 ℃~800 ℃ heat treatments, interior pipe strong bond is made composite ceramic protecting pipe in outer tube.
In the said method, described composite SiC ceramic material comprises following component: SiC40~70% by mass percentage; Al 2O 35~10%; CaO5~10%; C10~50%.Described composite S i 3N 4Coat comprises following component: Si by mass percentage 3N 450~85%; Al 2O 35~20%; Y 2O 310~30%.Described SiC ceramic based material comprises following component: SiC70~85% by mass percentage; Al 2O 35~10%; Si 5~10%; C5~10%.Described AlN ceramic based material comprises following component: AlN70~85% by mass percentage; Al 2O 310~20%; Y 2O 35~10%.Described low melting point ceramic glaze comprises following component: SiO by mass percentage 260~70%; Al 2O 37~10%; B 2O 35~10%; K 2O+Na 2O5~8%; CaO 5~10%; ZnO3~7%.
The ceramic outer tube of composite ceramic protecting pipe of the present invention adopt do not soak into, non-leakage, do not corrode the indehiscent composite SiC material preparation of anti-rapid heat cycle and mantle surface applies; ceramic inner pipe adopts high temperature resistant; AlN or SiC sill anti-oxidant, high-strength, high heat conduction prepare; and by low melting point ceramic glaze bonding transition zone between inner and outer pipe; can fine shutoff outer tube higher porosity, guarantee the good combination of inner and outer pipe.Can satisfy protection tube and metal liquid does not soak into, does not leak, do not corrode by inside and outside two kinds of different materials potteries compound, thermal shock drag height, the requirement of combination property such as chilling and shock heating does not ftracture, and thermal conductance is good has the intensity height, the advantage that the life-span is long.
Description of drawings
Fig. 1 is the structure chart of composite ceramic protecting pipe of the present invention.Among the figure: 1, outer tube; 2, interior pipe; 3, bonding transition zone; 4, outer tube surface coating layer; 5, heater element.
Embodiment
The present invention is described in further detail below in conjunction with drawings and the specific embodiments.
As shown in Figure 1, immersion type hot-dip plating composite ceramic protecting pipe of the present invention comprises the composite SiC pottery outer tube 1 that an end seals, and this outer tube is provided with composite S i outward 3N 4Coat 4 is bonded with pipe 2 in SiC or the AlN pottery in this outer tube, Guan Yiduan external shape just matches with the interior shape that outer tube 1 seals an end in this, in the interior pipe 2 heater element 5 can be installed, and heater element can adopt Elema or Si-Mo rod.Bonding transition zone 3 is the low melting point ceramic glaze between outer tube and interior pipe.
Pottery outer tube 1 is because will (Mg) liquid directly contacts for Al, Zn, therefore requires material to possess preventing corrosion from molten metals, and the life-span grows, do not soak into, non-leakage, anti-thermal shock, do not ftracture with high-temperature metal.
According to above requirement, outer tube 1 material of the present invention adopts the composite SiC material, and its specific embodiment composition and preparation technology are as shown in table 1.
Table 1 outer tube ceramic formula
Figure GSA00000022169000031
Soak into and infiltration the composite S i on the outer tube of the present invention for improving outer tube 1 anti-metal 3N 4The specific embodiment of coat 4 is as shown in table 2.Coat 4 is to carry out on the plain embryo after outer tube 1 moulding, and the coating back is with outer tube 1 sintering.
The outer tube outer surface coat prescription of table 2 (quality %)
Become ??Si 3N 4 ??Al 2O 3 ??Y 2O 3
Be coated with 1 ??50 ??20 ??30
Be coated with 2 ??70 ??10 ??20
Be coated with 3 ??85 ??5 ??10
In the ceramic inner pipe 2 heater element 5 will be installed, so require material to possess: high temperature resistant, anti-oxidant, for this reason, pipe 1 material adopts SiC or compound AlN material in the present invention, its specific embodiment form and preparation technology as shown in table 3.
In order to guarantee the good combination of outer tube 1 and interior pipe 2, remedy outer tube remain higher porosity, the bonding transition zone 3 of interior pipe 2 and outer tube 1 adopt can sealing of hole low melting point ceramic glaze material, it specifically fills a prescription as shown in table 4.In ceramic glaze is coated in will showing in the outer or outer tube of pipe, fit into interior pipe in the outer tube after, in 700 ℃~800 ℃ heat treatments, but just sealing of hole and interior pipe 2 firmly is compounded in the outer tube 1.
Pipe ceramic formula in the table 3
Figure GSA00000022169000041
Table 4 bonding transition zone prescription (quality %)
Become ??SiO 2 ??Al 2O 3 ??B 2O 3 ??K 2O+Na 2O ??CaO ??ZnO
Glaze 1 ??60 ??10 ??5 ??8 ??10 ??7
Glaze 2 ??70 ??7 ??10 ??5 ??5 ??3
The outer tube (coat is " being coated with 1 ") that will consist of " outer 1 " is by bonding transition zone " glaze 1 " and the compound multiple tube 1 of making of interior pipe that consists of " interior 1 ".
The outer tube (coat is " being coated with 2 ") that will consist of " outer 2 " is by bonding transition zone " glaze 2 " and the compound multiple tube of making of interior pipe that consists of " interior 2 ".
The outer tube (coat is " being coated with 3 ") that will consist of " outer 3 " is by bonding transition zone " glaze 1 " and the compound multiple tube 3 of making of interior pipe that consists of " interior 3 ".
More than the performance of three kinds of composite ceramic protecting pipes referring to table 5
Table 5 composite ceramic protecting pipe The performance test results of the present invention
Code name Use molten non-ferrous metal Chilling and shock heating Thermal shock drag (Tc/ ℃) Life-span (moon)
Multiple tube 1 Al, Mg, Zn, Cu etc. Do not ftracture ?1500 ??>6
Multiple tube 2 ??Al,Zn Do not ftracture ?1200 ??>18
Multiple tube 3 ??Zn Do not ftracture ?1000 ??>18

Claims (7)

1. an immersion type hot-dip plating composite ceramic protecting pipe is characterized in that, comprises the composite SiC pottery outer tube of end sealing, and this outer tube outer wall is provided with composite S i 3N 4Coat is provided with pipe in SiC or the AlN base pottery in this outer tube, described interior Guan Yiduan is used to install the heater element that stretches into wherein; The other end external shape of interior pipe just matches with the interior shape of outer duct occlusion one end; Be low melting point ceramic glaze bonding transition zone between described outer tube and interior pipe.
2. the preparation method of the described immersion type hot-dip plating composite ceramic protecting pipe of claim 1 is characterized in that, comprises the steps:
(1) prepares the outer tube biscuit that an end seals with the composite SiC ceramic material with the isostatic compaction method;
(2) coating composite S i on the outer tube biscuit 3N 4Coat, coat gets composite SiC pottery outer tube with outer tube biscuit 1450~1600 ℃ of sintering under nitrogen protection;
(3) prepare the interior pipe biscuit of end sealing with extruding or isostatic compaction method with SiC or AlN base ceramic material, 1450~1600 ℃ of reaction-sintereds get pipe in SiC or the AlN base pottery, and the external shape of Guan Yiduan just matches with the interior shape of outer duct occlusion one end of pottery in this pottery;
(4) the low melting point ceramic glaze is coated in step (2) the gained outer tube or step (3) gained in outside the pipe, fit into interior pipe in the outer tube after, in 700 ℃~800 ℃ heat treatments, interior pipe strong bond is made composite ceramic protecting pipe in outer tube.
3. as the preparation method of immersion type hot-dip plating composite ceramic protecting pipe as described in the claim 2, it is characterized in that described composite SiC ceramic material comprises following component: SiC40~70% by mass percentage; Al 2O 35~10%; CaO5~10%; C10~50%.
4. as the preparation method of immersion type hot-dip plating composite ceramic protecting pipe as described in the claim 3, it is characterized in that described composite S i 3N 4Coat comprises following component: Si by mass percentage 3N 450~85%; Al 2O 35~20%; Y 2O 310~30%.
5. as the preparation method of immersion type hot-dip plating composite ceramic protecting pipe as described in the claim 2, it is characterized in that described SiC ceramic based material comprises following component: SiC70~85% by mass percentage; Al 2O 35~10; Si 5~10%; C5~10%.
6. as the preparation method of immersion type hot-dip plating composite ceramic protecting pipe as described in the claim 2, it is characterized in that described AlN ceramic based material comprises following component: AlN70~85% by mass percentage; Al 2O 310~20%; Y 2O 35~10%.
7. as the preparation method of immersion type hot-dip plating composite ceramic protecting pipe as described in one of claim 2~6, it is characterized in that described low melting point ceramic glaze comprises following component: SiO by mass percentage 260~70%; Al 2O 37~10%; B 2O 35~10%; K 2O+Na 2O 5~8%; CaO 5~10%; ZnO 3~7%.
CN2010101041903A 2010-02-02 2010-02-02 Immersion type hot-dip plating composite ceramic protecting pipe and preparation method thereof Expired - Fee Related CN101765255B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102506429A (en) * 2011-11-07 2012-06-20 西安交通大学 Immersed gas ceramic inner heater sleeve and preparation method thereof
CN104219806A (en) * 2014-07-01 2014-12-17 长安大学 Liquid-interlayer ceramic-metal composite bushing for immersion heater and manufacturing method of bushing
CN105509488A (en) * 2015-12-23 2016-04-20 西安超码科技有限公司 Internal heating device with immersive ceramic resistor
CN106083066A (en) * 2016-06-12 2016-11-09 辽宁伊菲科技股份有限公司 Silicon nitride adds the manufacture method of heat pipe
CN111366215A (en) * 2020-04-09 2020-07-03 长春锅炉仪表程控设备股份有限公司 Composite ceramic electrode

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06228722A (en) * 1992-12-18 1994-08-16 Praxair St Technol Inc Melting resistant metal eroding sealing material and production thereof
CN2443005Y (en) * 2000-09-07 2001-08-15 吴金盛 Hot-dip equipment for wire straight-line moving into it through fusion pot
CN1387016A (en) * 2002-04-02 2002-12-25 上海交通大学 Heater coated with non-crystal viscose glass enamel
CN201390777Y (en) * 2008-08-01 2010-01-27 王青松 Heating rod of internal heating type hot-dip galvanized device

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102506429A (en) * 2011-11-07 2012-06-20 西安交通大学 Immersed gas ceramic inner heater sleeve and preparation method thereof
CN102506429B (en) * 2011-11-07 2013-12-04 西安交通大学 Immersed gas ceramic inner heater sleeve and preparation method thereof
CN104219806A (en) * 2014-07-01 2014-12-17 长安大学 Liquid-interlayer ceramic-metal composite bushing for immersion heater and manufacturing method of bushing
CN104219806B (en) * 2014-07-01 2016-01-06 长安大学 A kind of immersion heater liquid intermediate layer ceramic-metal cladding sleeve pipe and manufacture method thereof
CN105509488A (en) * 2015-12-23 2016-04-20 西安超码科技有限公司 Internal heating device with immersive ceramic resistor
CN106083066A (en) * 2016-06-12 2016-11-09 辽宁伊菲科技股份有限公司 Silicon nitride adds the manufacture method of heat pipe
CN111366215A (en) * 2020-04-09 2020-07-03 长春锅炉仪表程控设备股份有限公司 Composite ceramic electrode

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