CN108341664A - Rare-earth oxide modified ceramic core composition and preparation method thereof - Google Patents
Rare-earth oxide modified ceramic core composition and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of rare-earth oxide modified ceramic core composition, including:By modified ceramic fiber, basalt fibre, mullite fiber, silica, zirconium oxide, magnesia, paraffin and terpene resin according to 100:5‑10:1‑5:200‑300:50‑60:20‑50:150‑300:100 200 weight ratio, which is mixed, obtains the rare-earth oxide modified ceramic core composition;Wherein, the modified ceramic fiber obtains after carrying out coupling agent solution, the processing of densification physical modification, pre-oxidation, low-temperature carbonization and high temperature cabonization successively by ceramic fibre.The rare-earth oxide modified ceramic core composition material is simple and abundance, and ceramic core has excellent tensile strength made from the composition.
Description
Technical field
The present invention relates to casting fields, and in particular, to a kind of rare-earth oxide modified ceramic core composition and its system
Preparation Method.
Background technology
The complicated inner cavity of alloy-steel casting is mainly molded by using prefabricated ceramic core, and is tried after casting is cast
Removing.Its technological process is as follows:Tao Xin preparations, the wax-pattern preparation containing Tao Xin, the dewaxing of shell processed, shell and roasting, take off alloy casting
Core.It is well known that as China develops the startup of large aircraft project and various new work engine research and development program elements, to titanium alloy fine
More stringent requirements are proposed for body, structure and its performance of close casting.
Currently, studying relatively broad silica, oxidation silicon-base ceramic core, molten titanium is closed because core material does not have
The good chemical reaction inertia of gold and core leach technics complexity is difficult to apply to titanium alloy fine casting field.Due to boron nitride and molten titanium
Alloy has higher chemical reaction inertia at high temperature, and has good high-temperature creep resistance, and boron nitride is a kind of very suitable
Share the aggregate for making titanium alloy fine casting ceramic core.The concern of related scientific research personnel, such as publication number are caused in recent years
200610028168.9 Chinese invention patent application disclose a kind of boron nitride ceramics for titanium or titanium alloy hot investment casting
The preparation method of shell uses boron nitride powder and its acetic acid zirconium or Ludox that painting slurry is made for binder in the invention.By
It becomes increasingly complex in the shape of titanium alloy, for present titanium alloy casting often with complicated inner cavity, this requires core in titanium alloy
Has the integrality of good high-temperature creep resistance and then guarantee shape in casting process while also to the detachability to core
More stringent requirements are proposed for energy.But boron nitride stable chemical performance brings certain difficulty especially for shape to core removing
Complicated core is difficult mechanically to be purged.In order to improve the depoling performance of core, type silicon oxide core material also by
The concern of related scientific research personnel, as the Chinese invention patent application of CN102531648A discloses a kind of Ti alloy casting oxidation
Silicon substrate ceramic core and preparation method are prepared since in titanium alloy precision casting, the process is more complicated from the wax-pattern containing Tao Xin
To alloy the duration of pouring generally at two weeks or more, core will be in contact in use with water based paint.Above-mentioned patent
The core prepared occurs hydration reaction and causes the defeated and dispersed of core after meeting water, and therefore, above-mentioned core is difficult to be applied to
Titanium alloy etc. needs the requirement of the core strength of high-accuracy casting field and ceramics is also relatively high to be difficult to meet.
Invention content
The object of the present invention is to provide a kind of rare-earth oxide modified ceramic core composition and preparation method thereof, the rare earths
Oxide modifying ceramic core composition material is simple and abundance, and ceramic core has excellent drawing made from the composition
Stretch intensity.
To achieve the goals above, the present invention provides a kind of preparation sides of rare-earth oxide modified ceramic core composition
Method, including:
By modified ceramic fiber, basalt fibre, mullite fiber, silica, zirconium oxide, magnesia, paraffin and terpenes
Resin is according to 100:5-10:1-5:200-300:50-60:20-50:150-300:The weight ratio of 100-200 is mixed to obtain the final product
To the rare-earth oxide modified ceramic core composition;Wherein, the modified ceramic fiber is coupled successively by ceramic fibre
With yttrium oxide ground and mixed after agent solution pretreatment, the processing of densification physical modification, pre-oxidation, cryogenic carbon are then carried out successively again
It is obtained after change and high temperature cabonization.
Rare-earth oxide modified ceramic core composition made from a kind of above-mentioned preparation method is additionally provided in the present invention.
Through the above technical solutions, selected in the present invention first by ceramic fibre after coupling agent pre-processes again with yttrium oxide
Ground and mixed is then carried out being densified physical modification processing, pre-oxidation, low-temperature carbonization and high temperature cabonization modification and then be obtained successively again
To modified ceramic fiber;Modified ceramic fiber, basalt fibre and mullite fiber are made according to specific weight proportion again
Raw material of the conjugate fiber as ceramic core, and mixed with raw materials such as silica, zirconium oxide, magnesia, paraffin and terpene resins
It closes and then rare-earth oxide modified ceramic core composition is made;Ceramic core made from the composition has excellent stretching strong
Degree.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific implementation mode
The specific implementation mode of the present invention is described in detail below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
A kind of preparation method of rare-earth oxide modified ceramic core composition is provided in the present invention, including:
By modified ceramic fiber, basalt fibre, mullite fiber, silica, zirconium oxide, magnesia, paraffin and terpenes
Resin is according to 100:5-10:1-5:200-300:50-60:20-50:150-300:The weight ratio of 100-200 is mixed to obtain the final product
To the rare-earth oxide modified ceramic core composition;Wherein, the modified ceramic fiber is carried out successively by ceramic fibre
It is obtained after the processing of densification physical modification, pre-oxidation, low-temperature carbonization and high temperature cabonization.
In above-mentioned technical proposal, the method for modifying of the modified ceramic fiber can there are many selections, but in order to improve
The tensile strength of modified ceramic fiber obtained, it is preferable that modified ceramic fiber is made by the following method:
1) by coupling agent and water according to 1:The weight ratio of 90-100 carries out being mixed to prepare treatment fluid;
2) ceramic fibre is put into the treatment fluid and is once impregnated, ground and is stirred;
3) then, be filtered, dry after be placed again into the treatment fluid carry out it is secondary immersion and filter, dry
To pretreatment ceramic fibre;
4) by above-mentioned pretreatment ceramic fibre and yttrium oxide according to 100:Mixture is made in the weight ratio grinding of 1-1.5, connects
It and obtains institute after the mixture to be carried out to the processing of densification physical modification, pre-oxidation, low-temperature carbonization and high temperature cabonization successively
State modified ceramic fiber.
In above-mentioned technical proposal, the condition of the densification physical modification processing can select in a wide range, still
In order to improve modified effect, it is preferable that densification physical modification processing at least meets the following conditions:In air medium, in
At a temperature of 140-200 DEG C, impose the drawing-offs of 0-+5% elongations, processing time 2-10min.
In above-mentioned technical proposal, the condition of the pre-oxidation treatment can select in a wide range, but in order to improve
Pre-oxidation, modified effect, it is preferable that the pre-oxidation at least meets the following conditions:In air medium, in 200-300 DEG C of temperature
Under degree, impose the drawing-offs of 0-+10% elongations, processing time 100-150min.
In above-mentioned technical proposal, the condition of the low-temperature carbonization processing can select in a wide range, but in order to carry
Height carbonization effect, it is preferable that the low-temperature carbonization at least meets the following conditions:Under the protection of nitrogen atmosphere, impose -3-+
The drawing-off of 10% elongation, be carbonized 2-10min at a temperature of 500-600 DEG C.
In above-mentioned technical proposal, the condition of the high temperature cabonization processing can select in a wide range, but in order to carry
Height carbonization effect, it is preferable that the high temperature cabonization at least meets the following conditions:Under the protection of nitrogen atmosphere, -3-+5% is imposed
Under the drawing-off of elongation, be carbonized 0.2-3min at a temperature of 1300-1350 DEG C.
In above-mentioned technical proposal, the type of the coupling agent can select in a wide range, but in order to improve pre- place
Manage the tensile strength of ceramic core made from effect and raisings the composition, it is preferable that the coupling agent be irrigate orchid inorganic agent,
The coupling agent that the trade mark is KH560 or the trade mark is KH550.
In above-mentioned technical proposal, the actual conditions of the immersion can select in a wide range, but in order to improve leaching
Steep effect and efficiency, it is preferable that the primary immersion and secondary impregnate separate at least meet the following conditions:Soaking temperature
It is 20-60 DEG C, soaking time 30-6min.
In above-mentioned technical proposal, the milling time, drying temperature can control in a wider scope, but in order to
Improve grinding, drying efficiency, it is preferable that wherein, the time of the grinding is 10-20min;
Drying temperature described in step 3) is 20-60 DEG C.
A kind of obtained rare-earth oxide modified ceramic core composition of above-mentioned preparation method is additionally provided in the present invention.
The present invention will be described in detail by way of examples below.
Embodiment 1
1) by fertile blue inorganic agent and water according to 1:90 weight ratio carries out being mixed to prepare treatment fluid;
2) ceramic fibre is put into the treatment fluid to grinding 10min after impregnating 60min at 30 DEG C and is stirred;
3) then, be filtered, at 30 DEG C dry after be placed again into the treatment fluid carry out it is secondary immersion (at 30 DEG C
Impregnate 60min) and filter, 60 DEG C drying obtain pretreatment ceramic fibre;
4) by above-mentioned pretreatment ceramic fibre and yttrium oxide according to 100:Mixture is made in 1 weight ratio grinding, then will
The mixture obtains described change after carrying out the processing of densification physical modification, pre-oxidation, low-temperature carbonization and high temperature cabonization successively
Property ceramic fibre, by the modified ceramic fiber and basalt fibre, mullite fiber, silica, zirconium oxide, magnesia, paraffin
With terpene resin according to 100:5:1:200:50:20:150:100 weight ratio, which is mixed, to be obtained the rare earth oxide and changes
Property ceramic core composition, is denoted as A1;
Wherein, the densification physical modification processing at least meets the following conditions:In air medium, in 140 DEG C of temperature
Under, impose the drawing-off of+1% elongation, processing time 10min;
Pre-oxidation at least meets the following conditions:In air medium, at a temperature of 200 DEG C, impose leading for+2% elongation
It stretches, processing time 150min;
Low-temperature carbonization at least meets the following conditions:Under the protection of nitrogen atmosphere, the drawing-off that imposes -3% elongation,
Be carbonized 10min at a temperature of 500 DEG C;
High temperature cabonization at least meets the following conditions:Under the protection of nitrogen atmosphere, impose under the drawing-off of+1% elongation,
Be carbonized 3min at a temperature of 1300 DEG C.
Corresponding rare earth is made according to the method for application examples 1 in rare-earth oxide modified ceramic core composition A1 obtained
Oxide modifying ceramic core is denoted as A1 ';It is 30MPa to measure its tensile strength at room temperature.
Embodiment 2
1) by coupling agent and water that the trade mark is KH560 according to 1:95 weight ratio carries out being mixed to prepare treatment fluid;
2) ceramic fibre is put into the treatment fluid to grinding 15min after impregnating 40min at 45 DEG C and is stirred;
3) then, be filtered, at 50 DEG C dry after be placed again into the treatment fluid carry out it is secondary immersion (at 45 DEG C
Impregnate 40min) and filter, 60 DEG C drying obtain pretreatment ceramic fibre;
4) by above-mentioned pretreatment ceramic fibre and yttrium oxide according to 100:Mixture is made in 1.2 weight ratio grinding, then
The mixture is carried out successively to obtain after the processing of densification physical modification, pre-oxidation, low-temperature carbonization and high temperature cabonization described
Modified ceramic fiber, by the modified ceramic fiber and basalt fibre, mullite fiber, silica, zirconium oxide, magnesia, stone
Wax and terpene resin are according to 100:8:3:250:55:30:250:150 weight ratio, which is mixed, obtains the rare earth oxide
Modified ceramic core composition, is denoted as A2;
Wherein, the densification physical modification processing at least meets the following conditions:In air medium, in 180 DEG C of temperature
Under, impose the drawing-off of+3% elongation, processing time 7min;
Pre-oxidation at least meets the following conditions:In air medium, at a temperature of 250 DEG C, impose leading for+5% elongation
It stretches, processing time 120min;
Low-temperature carbonization at least meets the following conditions:Under the protection of nitrogen atmosphere, the drawing-off that imposes+5% elongation,
Be carbonized 6min at a temperature of 550 DEG C;
High temperature cabonization at least meets the following conditions:Under the protection of nitrogen atmosphere, impose under the drawing-off of+5% elongation,
Be carbonized 1.5min at a temperature of 1330 DEG C.
Corresponding rare earth is made according to the method for application examples 1 in rare-earth oxide modified ceramic core composition A2 obtained
Oxide modifying ceramic core is denoted as A2 ';It is 28MPa to measure its tensile strength at room temperature.
Embodiment 3
1) by coupling agent and water that the trade mark is KH550 according to 1:100 weight ratio carries out being mixed to prepare treatment fluid;
2) ceramic fibre is put into the treatment fluid to grinding 15min after impregnating 40min at 60 DEG C and is stirred;
3) then, be filtered, at 50 DEG C dry after be placed again into the treatment fluid carry out it is secondary immersion (at 60 DEG C
Impregnate 40min) and filter, 60 DEG C drying obtain pretreatment ceramic fibre;
4) by above-mentioned pretreatment ceramic fibre and yttrium oxide according to 100:Mixture is made in 1.5 weight ratio grinding, then
The mixture is carried out successively to obtain after the processing of densification physical modification, pre-oxidation, low-temperature carbonization and high temperature cabonization described
Modified ceramic fiber, by the modified ceramic fiber and basalt fibre, mullite fiber, silica, zirconium oxide, magnesia, stone
Wax and terpene resin are according to 100:10:5:300:60:50:300:200 weight ratio, which is mixed, obtains the rare-earth oxidation
Object modified ceramic core composition, is denoted as A3;
Wherein, the densification physical modification processing at least meets the following conditions:In air medium, in 200 DEG C of temperature
Under, impose the drawing-off of+1% elongation, processing time 2min;
Pre-oxidation at least meets the following conditions:In air medium, at a temperature of 300 DEG C, impose leading for+10% elongation
It stretches, processing time 100min;
Low-temperature carbonization at least meets the following conditions:Under the protection of nitrogen atmosphere, the drawing-off that imposes+10% elongation,
Be carbonized 2min at a temperature of 600 DEG C;
High temperature cabonization at least meets the following conditions:Under the protection of nitrogen atmosphere, impose under the drawing-off of+5% elongation,
Be carbonized 0.2min at a temperature of 1350 DEG C.
Corresponding rare earth is made according to the method for application examples 1 in rare-earth oxide modified ceramic core composition A3 obtained
Oxide modifying ceramic core is denoted as A3 ';It is 27MPa to measure its tensile strength at room temperature.
Comparative example 1
Rare-earth oxide modified ceramic core composition is prepared Following the procedure of Example 1, is denoted as D1;The difference is that right
Sour aluminium ceramic fibre is not right before successively carrying out the processing of densification physical modification, pre-oxidation, low-temperature carbonization and high temperature cabonization successively
Ceramic fibre carries out the pretreatment for the treatment of fluid immersion.
Corresponding rare earth is made according to the method for application examples 1 in rare-earth oxide modified ceramic core composition D1 obtained
The D1 ' that oxide modifying ceramic core is denoted as;It is 18MPa to measure its tensile strength at room temperature.
Comparative example 2
Rare-earth oxide modified ceramic core composition is prepared Following the procedure of Example 1, is denoted as D2;Unlike not into
Row densification physical modification processing.
Corresponding rare earth is made according to the method for application examples 1 in rare-earth oxide modified ceramic core composition D2 obtained
The D2 ' that oxide modifying ceramic core is denoted as;It is 17MPa to measure its tensile strength at room temperature.
Comparative example 3
Rare-earth oxide modified ceramic core composition is prepared Following the procedure of Example 1, is denoted as D3;Unlike not into
Row pre-oxidation treatment.
Corresponding rare earth is made according to the method for application examples 1 in rare-earth oxide modified ceramic core composition D3 obtained
The D3 ' that oxide modifying ceramic core is denoted as;It is 17MPa to measure its tensile strength at room temperature.
Comparative example 4
Rare-earth oxide modified ceramic core composition is prepared Following the procedure of Example 1, is denoted as D4;Unlike not into
Row low-temperature carbonization.
Corresponding rare earth is made according to the method for application examples 1 in rare-earth oxide modified ceramic core composition D4 obtained
The D4 ' that oxide modifying ceramic core is denoted as;It is 15MPa to measure its tensile strength at room temperature.
Comparative example 5
Rare-earth oxide modified ceramic core composition is prepared Following the procedure of Example 1, is denoted as D5;Unlike not into
Row high temperature cabonization.
Corresponding rare earth is made according to the method for application examples 1 in rare-earth oxide modified ceramic core composition D5 obtained
The D5 ' that oxide modifying ceramic core is denoted as;It is 14MPa to measure its tensile strength at room temperature.
Comparative example 6
Rare-earth oxide modified ceramic core composition is prepared Following the procedure of Example 1, is denoted as D6;The difference is that step
4) yttrium oxide mixing is not added in.
Corresponding rare earth is made according to the method for application examples 1 in rare-earth oxide modified ceramic core composition D5 obtained
The D5 ' that oxide modifying ceramic core is denoted as;It is 22MPa to measure its tensile strength at room temperature.
Application examples 1
By modified ceramic fiber respectively with basalt fibre, mullite fiber, silica, zirconium oxide, magnesia, paraffin and
Terpene resin is according to 100:5-10:1-5:200-300:50-60:20-50:150-300:The weight ratio of 100-200 mixed,
Heating stirring obtains slurry;The slurry is injected in ceramic core mold and carries out pressure injection, high-temperature roasting is then carried out and pottery is made
Porcelain core idiosome;Finally, corresponding rare earth oxide is made in drying after the ceramic core idiosome being immersed in silicon sol solution
Modified ceramic core is denoted as A1 '-A3 ' and D1 '-D6 '.
In addition, testing above-mentioned obtained rare-earth oxide modified ceramic core according to GB/t23805-2009 is denoted as A1 '-A3 '
And tensile strengths (MPa) of the D1 '-D6 ' at 25 DEG C of room temperature;Concrete outcome is shown in that embodiment is recorded.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of preparation method of rare-earth oxide modified ceramic core composition, which is characterized in that including:
By modified ceramic fiber, basalt fibre, mullite fiber, silica, zirconium oxide, magnesia, paraffin and terpene resin
According to 100:5-10:1-5:200-300:50-60:20-50:150-300:The weight ratio of 100-200, which is mixed, obtains institute
State rare-earth oxide modified ceramic core composition;
Wherein, the modified ceramic fiber be by ceramic fibre successively coupling agent solution pre-process after with yttrium oxide ground and mixed,
Then carry out what densification physical modification was handled, and pre-oxidized, being obtained after low-temperature carbonization and high temperature cabonization successively again.
2. preparation method according to claim 1, wherein the modified ceramic fiber is made by the following method:
1) by coupling agent and water according to 1:The weight ratio of 90-100 carries out being mixed to prepare treatment fluid;
2) ceramic fibre is put into the treatment fluid and is once impregnated, ground and is stirred;
3) then, be filtered, dry after be placed again into the treatment fluid carry out it is secondary immersion and filter, dry obtain it is pre-
Handle ceramic fibre;
4) by above-mentioned pretreatment ceramic fibre and yttrium oxide according to 100:Mixture is made in the weight ratio grinding of 1-1.5, then will
The mixture obtains described change after carrying out the processing of densification physical modification, pre-oxidation, low-temperature carbonization and high temperature cabonization successively
Property ceramic fibre.
3. preparation method according to claim 2, wherein the densification physical modification processing at least meets following item
Part:In air medium, at a temperature of 140-200 DEG C, impose the drawing-offs of 0-+5% elongations, processing time 2-10min.
4. preparation method according to claim 2, wherein the pre-oxidation at least meets the following conditions:In air dielectric
In, at a temperature of 200-300 DEG C, impose the drawing-offs of 0-+10% elongations, processing time 100-150min.
5. preparation method according to claim 2, wherein the low-temperature carbonization at least meets the following conditions:In nitrogen gas
Under the protection of atmosphere, the drawing-off that imposes -3-+10% elongations, be carbonized 2-10min at a temperature of 500-600 DEG C.
6. preparation method according to claim 2, wherein the high temperature cabonization at least meets the following conditions:In nitrogen gas
It under the protection of atmosphere, imposes under the drawing-off of -3-+5% elongations, be carbonized 0.2-3min at a temperature of 1300-1350 DEG C.
7. preparation method according to claim 2, wherein the coupling agent is fertile blue inorganic agent, the trade mark is KH560 or board
Number be KH550 coupling agent.
8. according to the preparation method described in any one of claim 2-7, wherein the primary immersion and secondary immersion are respective
It is independent at least to meet the following conditions:Soaking temperature is 20-60 DEG C, soaking time 30-6min.
9. according to the preparation method described in any one of claim 2-7, wherein the time of the grinding is 10-20min;
Drying temperature described in step 3) is 20-60 DEG C.
10. rare-earth oxide modified ceramic core group is made in a kind of preparation method by described in any one of claim 1-9
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110306131A (en) * | 2019-06-28 | 2019-10-08 | 重庆电子工程职业学院 | A kind of composite material of magnesium alloy and preparation method thereof |
CN113354422A (en) * | 2020-03-04 | 2021-09-07 | 中国科学院金属研究所 | Ceramic core for single crystal high-temperature alloy blade and preparation method thereof |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110306131A (en) * | 2019-06-28 | 2019-10-08 | 重庆电子工程职业学院 | A kind of composite material of magnesium alloy and preparation method thereof |
CN110306131B (en) * | 2019-06-28 | 2021-04-23 | 重庆电子工程职业学院 | Magnesium alloy composite material and preparation method thereof |
CN113354422A (en) * | 2020-03-04 | 2021-09-07 | 中国科学院金属研究所 | Ceramic core for single crystal high-temperature alloy blade and preparation method thereof |
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