CN104072156B - A kind of Nano-compound Ceramic Core - Google Patents

A kind of Nano-compound Ceramic Core Download PDF

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CN104072156B
CN104072156B CN201410224822.8A CN201410224822A CN104072156B CN 104072156 B CN104072156 B CN 104072156B CN 201410224822 A CN201410224822 A CN 201410224822A CN 104072156 B CN104072156 B CN 104072156B
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nano
rare earth
ceramic core
composite granule
powder
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CN104072156A (en
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高博
王伟
姜银珠
赵夫涛
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Zhejiang Zhenxing Axiang Group Co ltd
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WUHU ZHEXIN NEW ENERGY CO Ltd
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Abstract

The invention discloses a kind of Nano-compound Ceramic Core, it is characterized in that what it was made up of the raw material of following weight per-cent: mineralizer 12-18wt%, softening agent 14-20wt%, nano silicon 2-3wt%, nano magnesia 1-2wt%, Microcrystalline Wax 2-3wt%, surplus is rare earth clad nano composite granule, ceramic core of the present invention has enough bending strengths, percent of firing shrinkage is little, the not variability of size and dimension can be ensured, because what adopt is the starting material of different fineness, effectively can improve the porosity of core, thus can be good at improving depoling performance.

Description

A kind of Nano-compound Ceramic Core
Technical field
The present invention relates generally to precision casting field, particularly relates to a kind of Nano-compound Ceramic Core.
Background technology
The complicated inner cavity of alloy-steel casting is shaping mainly through using prefabricated ceramic core, and manages to remove after foundry goods is cast.Its technical process is as follows: prepared by Tao Xin, prepare containing the wax-pattern of Tao Xin, the dewaxing of shell processed, shell and roasting, alloy casting, depoling.As everyone knows, along with China's development large aircraft project and the startup of various new work engine research and development program element, the body of titanium alloy precision casting, structure and performance thereof are had higher requirement.
At present, research magnesium oxide, silicon oxide base ceramic core comparatively widely, because core material does not possess the good chemical reaction inertia of molten titanium alloy and core leach technics complexity is difficult to be applied to titanium alloy fine casting field.With molten titanium alloy, at high temperature there is higher chemical reaction inertia due to nano combined, and the high-temperature creep resistance that tool is good, nano combined is a kind of aggregate being well suited for being used as titanium alloy fine casting ceramic core.Cause the concern of related scientific research personnel in recent years, Chinese invention patent application as publication number 200610028168.9 discloses a kind of preparation method of the nano composite ceramic shell for titanium or titanium alloy precision casting, adopts nano composite powder and acetic acid zirconium or silicon sol thereof to be that painting slip made by binding agent in this invention.Because the shape of titanium alloy becomes increasingly complex, present titanium alloy casting is often with complicated inner cavity, and this requires core in titanium alloy casting process, possess good high-temperature creep resistance and then ensures that the integrity of shape is also had higher requirement to the performance that removes of core simultaneously.But nano combined stable chemical performance to core remove bring certain difficulty especially for complex-shaped core be difficult to mechanically remove.In order to improve the depoling performance of core, magnesium oxide core material also receives the concern of related scientific research personnel, Chinese invention patent application as CN102531648A discloses a kind of nano composite oxides magnesium matrix ceramic core and preparation method, due to comparatively complicated in titanium alloy precision casting technique, be prepared into the duration of pouring of alloy generally all more than two weeks from the wax-pattern containing Tao Xin, core in use will contact with water-based paint.Namely hydration reaction occur after the core that above-mentioned patent is prepared meets water and cause the defeated and dispersed of core, therefore, above-mentioned core is difficult to be applied to titanium alloy precision casting field.
Summary of the invention
The object of the invention is just to provide a kind of Nano-compound Ceramic Core.
The present invention is achieved by the following technical solutions:
A kind of Nano-compound Ceramic Core, is characterized in that what it was made up of the raw material of following weight per-cent:
Mineralizer 12-18wt%, softening agent 14-20wt%, nano silicon 2-3wt%, nano magnesia 1-2wt%, Microcrystalline Wax 2-3wt%, surplus are rare earth clad nano composite granule;
Described mineralizer be one in zirconium dioxide, calcium oxide, silicon-dioxide or two kinds and more than, with any mass ratio mixing composition;
Described softening agent is made up of the raw material of following weight parts:
Paraffin 82-90, propolis 3-4, alumino silica gel 6-8, sebacic acid propanediol polyester 1-2, aluminium hydrate powder 2-3, Silane coupling agent KH550 0.1-0.2;
Above-mentioned heating paraffin is melted, adds propolis, aluminium hydrate powder, Silane coupling agent KH550,300-400 rev/min of dispersed with stirring 10-12 minute, add each raw material of residue, stir, at 80-90 DEG C, insulation leaves standstill 3-5 minute, cooling discharging, obtains described softening agent;
The preparation method of described rare earth clad nano composite granule comprises the following steps:
(1) by nano aluminium oxide, nano silicon mixing, join in 100-200 times of deionized water, ultrasonic disperse, obtains dispersion liquid;
(2) boron nitride powder is mixed with calcium chloride, add Silane coupling agent KH550,1600-2000 rev/min of dispersed with stirring 10-15 minute, ball milling, dry, obtain particle diameter 60-150 μm, obtain basic powder;
(3) join in upper dispersion liquid by basic powder, dispersed with stirring, obtains premixed liquid;
(4) by inorganic zirconium salts and inorganic yttrium salts using any ratio mixing as rare earth oxide presoma, take inorganic zirconium salts and inorganic yttrium salts and put into the container filling deionized water and stirs and heat and obtain precursor solution;
(5) add in precursor solution by above-mentioned premixed liquid, the pH value of regulator solution, to 8-10, obtains mixed solution;
(6) dried by above-mentioned mixed solution, obtain drying powder, oven dry powder is carried out sintering and obtain rare earth clad nano composite granule, sintering temperature is 1200-1500 DEG C, and the time is 0.5-20h.
2, a kind of Nano-compound Ceramic Core according to claim 1, is characterized in that, in the preparation of described rare earth clad nano composite granule, the mixing quality of described rare earth oxide presoma and the mass ratio of basic powder are 1:24-30.
3, a kind of Nano-compound Ceramic Core according to claim 1, is characterized in that, in the preparation of described rare earth clad nano composite granule, described inorganic zirconium salts is zirconium chloride or zirconium nitrate, and described inorganic yttrium salts is Yttrium trichloride or Yttrium trinitrate.
4, a kind of Nano-compound Ceramic Core according to claim 1, is characterized in that, in the preparation of described rare earth clad nano composite granule, described rare earth oxide precursor solution, its concentration is 0.01-0.4mol/L.
5, a kind of Nano-compound Ceramic Core according to claim 1, it is characterized in that, in the preparation of described rare earth clad nano composite granule, the mass ratio of described boron nitride powder and nano silicon, nano aluminium oxide, calcium chloride is 100:4-5:5-6:2-3.
6, a preparation method for Nano-compound Ceramic Core as claimed in claim 1, is characterized in that comprising the following steps:
(1) by above-mentioned nano silicon, nano magnesia, Microcrystalline Wax mixing, heated and stirred 10-15 minute at 50-60 DEG C, adds the 6-10% of above-mentioned rare earth clad nano composite granule weight, and ball milling is abundant, obtains Preblend;
(2) mixer is heated to 120-140 DEG C, add softening agent, then each raw material of residue is added under agitation, continue after adding to be uniformly mixed 10-12 hour, carry out moulding as requested, sinter and obtain described Nano-compound Ceramic Core, described sintering temperature is 1300-1600 DEG C, and the time is 0.5-20h.
Advantage of the present invention is:
Ceramic core of the present invention has enough bending strengths, percent of firing shrinkage is little, can ensure the not variability of size and dimension, because what adopt is the starting material of different fineness, effectively can improve the porosity of core, thus can be good at improving depoling performance.
Embodiment
Embodiment 1
A kind of Nano-compound Ceramic Core, it is made up of the raw material of following weight per-cent:
Mineralizer 18wt%, softening agent 20wt%, nano silicon 3wt%, nano magnesia 2wt%, Microcrystalline Wax 3wt%, surplus are rare earth clad nano composite granule;
Described mineralizer is the mass ratio mixing compositions such as zirconium dioxide, calcium oxide, silicon-dioxide;
Described softening agent is made up of the raw material of following weight parts:
Paraffin 82, propolis 4, alumino silica gel 8, sebacic acid propanediol polyester 2, aluminium hydrate powder 3, Silane coupling agent KH550 0.2;
Above-mentioned heating paraffin melted, add propolis, aluminium hydrate powder, Silane coupling agent KH550,400 revs/min of dispersed with stirring 12 minutes, add each raw material of residue, stir, at 90 DEG C, insulation leaves standstill 3-5 minute, and cooling discharging, obtains described softening agent;
The preparation method of described rare earth clad nano composite granule comprises the following steps:
(1) by nano aluminium oxide, nano silicon mixing, join in 200 times of deionized waters, ultrasonic disperse, obtains dispersion liquid;
(2) boron nitride powder is mixed with calcium chloride, add Silane coupling agent KH550,2000 revs/min of dispersed with stirring 15 minutes, ball milling, dry, obtain particle diameter 150 μm, obtain basic powder;
(3) join in upper dispersion liquid by basic powder, dispersed with stirring, obtains premixed liquid;
(4) by inorganic zirconium salts and inorganic yttrium salts using any ratio mixing as rare earth oxide presoma, take inorganic zirconium salts and inorganic yttrium salts and put into the container filling deionized water and stirs and heat and obtain precursor solution;
(5) above-mentioned premixed liquid is added in precursor solution, the pH value to 10 of regulator solution, obtain mixed solution;
(6) dried by above-mentioned mixed solution, obtain drying powder, oven dry powder is carried out sintering and obtain rare earth clad nano composite granule, sintering temperature is 1500 DEG C, and the time is 10h.
A kind of Nano-compound Ceramic Core, in the preparation of described rare earth clad nano composite granule, the mixing quality of described rare earth oxide presoma and the mass ratio of basic powder are 1:30.
A kind of Nano-compound Ceramic Core, in the preparation of described rare earth clad nano composite granule, described inorganic zirconium salts is zirconium chloride or zirconium nitrate, and described inorganic yttrium salts is Yttrium trichloride or Yttrium trinitrate.
A kind of Nano-compound Ceramic Core, in the preparation of described rare earth clad nano composite granule, described rare earth oxide precursor solution, its concentration is 0.4mol/L.
A kind of Nano-compound Ceramic Core, in the preparation of described rare earth clad nano composite granule, the mass ratio of described boron nitride powder and nano silicon, nano aluminium oxide, calcium chloride is 100:5:6:2.
A preparation method for Nano-compound Ceramic Core, comprises the following steps:
(1) by above-mentioned nano silicon, nano magnesia, Microcrystalline Wax mixing, heated and stirred 15 minutes at 60 DEG C, adds 10% of above-mentioned rare earth clad nano composite granule weight, and ball milling is abundant, obtains Preblend;
(2) mixer is heated to 140 DEG C, adds softening agent, then add each raw material of residue under agitation, continue after adding to be uniformly mixed 12 hours, carry out moulding as requested, sinter and obtain described Nano-compound Ceramic Core, described sintering temperature is 1300 DEG C, and the time is 7h.
Performance test:
Room temperature bending strength 59MPa, high temperature amount of deflection (being incubated 30min at 1550 DEG C) 0.43mm, percent of firing shrinkage 0.55%.

Claims (5)

1. a Nano-compound Ceramic Core, is characterized in that it is made up of the raw material of following weight per-cent: mineralizer 12-18wt%, softening agent 14-20wt%, nano silicon 2-3wt%, nano magnesia 1-2wt%, Microcrystalline Wax 2-3wt%, surplus are rare earth clad nano composite granule;
Described mineralizer is one in zirconium dioxide, calcium oxide, silicon-dioxide or two or more, with any mass ratio mixing composition;
Described softening agent is made up of the raw material of following weight parts: paraffin 82-90, propolis 3-4, alumino silica gel 6-8, sebacic acid propanediol polyester 1-2, aluminium hydrate powder 2-3, Silane coupling agent KH550 0.1-0.2; Above-mentioned heating paraffin is melted, adds propolis, aluminium hydrate powder, Silane coupling agent KH550,300-400 rev/min of dispersed with stirring 10-12 minute, add each raw material of residue, stir, at 80-90 DEG C, insulation leaves standstill 3-5 minute, cooling discharging, obtains described softening agent;
The preparation method of described rare earth clad nano composite granule comprises the following steps:
(1) by nano aluminium oxide, nano silicon mixing, join in 100-200 times of deionized water, ultrasonic disperse, obtains dispersion liquid;
(2) boron nitride powder is mixed with calcium chloride, add Silane coupling agent KH550,1600-2000 rev/min of dispersed with stirring 10-15 minute, ball milling, dry, obtain the basic powder of particle diameter 60-150 μm;
(3) join in upper dispersion liquid by basic powder, dispersed with stirring, obtains premixed liquid;
(4) by inorganic zirconium salts and inorganic yttrium salts using any ratio mixing as rare earth oxide presoma, take inorganic zirconium salts and inorganic yttrium salts and put into the container filling deionized water and stirs and heat and obtain rare earth oxide precursor solution;
(5) add in precursor solution by above-mentioned premixed liquid, the pH value of regulator solution, to 8-10, obtains mixed solution;
(6) dried by above-mentioned mixed solution, obtain drying powder, oven dry powder is carried out sintering and obtain rare earth clad nano composite granule, sintering temperature is 1200-1500 DEG C, and the time is 0.5-20h.
2. a kind of Nano-compound Ceramic Core according to claim 1, is characterized in that, in the preparation of described rare earth clad nano composite granule, the mixing quality of described rare earth oxide presoma and the mass ratio of basic powder are 1:24-30.
3. a kind of Nano-compound Ceramic Core according to claim 1, is characterized in that, in the preparation of described rare earth clad nano composite granule, described inorganic zirconium salts is zirconium chloride or zirconium nitrate, and described inorganic yttrium salts is Yttrium trichloride or Yttrium trinitrate.
4. a kind of Nano-compound Ceramic Core according to claim 1, it is characterized in that, in the preparation of described rare earth clad nano composite granule, the mass ratio of described boron nitride powder and nano silicon, nano aluminium oxide, calcium chloride is 100:4-5:5-6:2-3.
5. a preparation method for Nano-compound Ceramic Core as claimed in claim 1, is characterized in that comprising the following steps:
(1) by above-mentioned nano silicon, nano magnesia, Microcrystalline Wax mixing, heated and stirred 10-15 minute at 50-60 DEG C, adds the 6-10% of above-mentioned rare earth clad nano composite granule weight, and ball milling is abundant, obtains Preblend;
(2) mixer is heated to 120-140 DEG C, add softening agent, then each raw material of residue is added under agitation, continue after adding to be uniformly mixed 10-12 hour, carry out moulding as requested, sinter and obtain described Nano-compound Ceramic Core, described sintering temperature is 1300-1600 DEG C, and the time is 0.5-20h.
CN201410224822.8A 2014-05-24 2014-05-24 A kind of Nano-compound Ceramic Core Expired - Fee Related CN104072156B (en)

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CN105418058B (en) * 2015-11-16 2017-12-12 沈阳黎明航空发动机(集团)有限责任公司 A kind of preparation method of low deformation toughness reinforcing silicon-base ceramic core

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1876272A (en) * 2006-06-27 2006-12-13 上海大学 Preparation method of boron nitride ceramic shell for titanium and titanium alloy precision casting
CN101537473A (en) * 2008-03-20 2009-09-23 上海市机械制造工艺研究所有限公司 Ceramic core for silica sol precision casting and manufacturing process thereof
EP2554294A2 (en) * 2011-08-03 2013-02-06 United Technologies Corporation Hybrid core assembly
CN102924062A (en) * 2012-10-25 2013-02-13 北京航空航天大学 Preparation method of calcium-oxide-based ceramic core

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1876272A (en) * 2006-06-27 2006-12-13 上海大学 Preparation method of boron nitride ceramic shell for titanium and titanium alloy precision casting
CN101537473A (en) * 2008-03-20 2009-09-23 上海市机械制造工艺研究所有限公司 Ceramic core for silica sol precision casting and manufacturing process thereof
EP2554294A2 (en) * 2011-08-03 2013-02-06 United Technologies Corporation Hybrid core assembly
CN102924062A (en) * 2012-10-25 2013-02-13 北京航空航天大学 Preparation method of calcium-oxide-based ceramic core

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Address before: 241000, No. 36 workshop of small and medium-sized enterprise park, South Zone, hi tech Industrial Development Zone, Yijiang District, Anhui, Wuhu

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