CN103159461A - Method for preparing calcium-oxide base ceramic core - Google Patents
Method for preparing calcium-oxide base ceramic core Download PDFInfo
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- CN103159461A CN103159461A CN2013100843309A CN201310084330A CN103159461A CN 103159461 A CN103159461 A CN 103159461A CN 2013100843309 A CN2013100843309 A CN 2013100843309A CN 201310084330 A CN201310084330 A CN 201310084330A CN 103159461 A CN103159461 A CN 103159461A
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Abstract
The invention relates to a method for preparing a calcium-oxide base ceramic core. The method comprises the following steps of: (1) preparing the blank of the calcium-oxide base ceramic core; (2) preparing a ZrO2/Y2O3 thin film on the surface of the blank of the calcium-oxide base ceramic core; and (3) carrying out enhanced sintering on the calcium-oxide base ceramic core. Because the surface of the blank of the pure calcium-oxide base ceramic core is coated with the film, the water resistance of the calcium-oxide base ceramic core is changed. Compared with the ceramic core in the prior art, the calcium-oxide base ceramic core is expanded in raw material and can be prepared from the pure calcium oxide. Because the surface of the blank of the pure calcium-oxide base ceramic core is coated with the nano film of the ZrO2/Y2O3 composite target material, the calcium-oxide base ceramic core can be protected against water and is easier to demould. The method provided by the invention is suitable for preparing the core in the precision casting process of titanium alloy.
Description
Technical field
The present invention is a kind of preparation method of calcium oxide-based ceramic core, belongs to the titanium alloy precision casting processing technique field.
Background technology
The complicated inner cavity of alloy-steel casting is mainly by coming moulding with prefabricated ceramic core, and manages to remove after foundry goods is cast.Its technical process is as follows: Tao Xin prepares, contains the wax-pattern preparation of Tao Xin, shell processed, shell dewaxing and roasting, alloy casting, depoling.Along with the startup of China's development large aircraft project and various new work engine research and development program elements, body and the structure of titanium alloy precision casting become increasingly complex, and often with complicated inner cavity, the especially depoling performance of over-all properties of core are had higher requirement.
At present, research aluminum oxide, silica-based ceramic core comparatively widely are not suitable for being applied to the titanium alloy fine casting field because core material does not possess to the good chemical reaction inertia of molten titanium alloy and depoling difficulty.Calcium oxide has caused related scientific research personnel's concern because having to the good chemical reaction inertia of molten titanium alloy and good depoling performance, disclose a kind of Ti alloy casting with calcium oxide matrix ceramic core and preparation method as the Chinese invention patent application of publication number CN 102531648 A, it includes the composition of following weight percent: 1.0～15% zirconium dioxide, 0.5～10.0% yttrium oxide, 0.05～0.1% Thorotrast and the calcium oxide of surplus.In this patent, the content of calcium oxide is 74.9～98.45wt%, due to comparatively complicated in titanium alloy precision casting technique, is prepared into duration of pouring of alloy from the wax-pattern that contains Tao Xin general all more than two weeks, and core in use will contact with water-based paint.Hydration reaction namely occurs and causes the defeated and dispersed of core after meeting water in core that above-mentioned patent is prepared, and therefore, above-mentioned core is difficult to be applied to the titanium alloy precision casting field.The Chinese invention patent application of publication number CN 1793033 A discloses a kind of titanium alloy precision casting ceramic core material, and the main body composition is zirconium white, and its content is 60～85wt%, and wherein the content of calcium oxide is 4～20wt%.At present, the depoling technique of core mainly contains: mechanical force is destroyed depoling, chemical corrosion depoling, mechanical force and is destroyed the depoling that combines with chemical corrosion, is difficult to carry out mechanical force destruction for the core of complicated shape and removes and can only adopt the chemical corrosion depoling method.In above-mentioned core, zirconic content is more, and zirconium white is again a kind of stable compound, is insoluble to acid-base solution, therefore, and the depoling of core difficulty, and owing to containing a certain amount of calcium oxide in core, core is faced with in use aquation problem equally.
Titanium alloy precision casting complex process, production cycle are longer, and core will contact with moisture coating in the operations such as shell processed, make core defeated and dispersed and can not continue to use and can generate pulverous calcium hydroxide after the suction of calcium oxide ceramics core.Therefore, a kind of calcium oxide powder with water resistant effect of exploitation is the needs in titanium industry actual production.
Summary of the invention
The present invention designs for above-mentioned the deficiencies in the prior art just a kind of calcium oxide-based ceramic core preparation method is provided, its objective is provides a kind of calcium oxide ceramics core that the molten titanium alloy is possessed the good chemical reactionlessness, and effectively reduce the hydration reaction that the calcium oxide ceramics core occurs in the process that contacts with water-based paint, thereby it is defeated and dispersed to prevent that core from occuring, realize simultaneously the chemical corrosion depoling, improve complicated inner cavity structure depoling performance.
The objective of the invention is to be achieved through the following technical solutions:
The preparation method of the calcium oxide-based ceramic core of this kind is characterized in that: the step of the method is:
⑴ prepare calcium oxide core blank
Chemical composition and the weight percent of calcium oxide core blank are: calcium oxide powder 85～95wt%, softening agent 5～15wt%, the chemical composition of described softening agent and weight percent are: paraffin 50～80wt%, beeswax 10～40wt%, oleic acid are 5～10wt%;
Take in proportion paraffin, beeswax and oleic acid, mix, obtain softening agent, take in proportion again calcium oxide powder and softening agent, mix, press sintering after the shape requirement moulding of core, sintering temperature is 900～1600 ℃, and sintering time is 0.5～20h, obtains calcium oxide core blank;
⑵ prepare ZrO in calcium oxide core blank surface
2/ Y
2O
3Film
At first use the calcium oxide-based ceramic core blank surface of sand papering, and with the cleaning of core blank, dry for standby, then with ZrO
2/ Y
2O
3Calcium oxide core blank (4) after composite target material (3) and surface treatment is placed in respectively main sputtering chamber (1) and the Sample Room (2) of magnetic control sputtering device, main sputtering chamber (1) and Sample Room (2) are vacuumized, when vacuum tightness reaches below 4 * 10-3Pa, to ZrO
2/ Y
2O
3Composite target material carries out pre-sputtering and removes its surface impurity, then rotating substrate rotating disk (5) makes the substrate on substrate rotating disk (5) be placed in aura, pass into argon gas to main sputtering chamber, adjustable pressure to 1 * 10-1～4 * 10-1Pa regulates calcium oxide core blank (4) and ZrO
2/ Y
2O
3The spacing of composite target material (3) is regulated sputtering power between 200～400W, build-up of luminance sputter, sputter 0.1～1h between 30～40mm.
(3) core is intensified-sintered
The surface is prepared ZrO
2/ Y
2O
3Film calcium oxide-based ceramic core later carries out intensified-sintered, and sintering temperature is 900～1600 ℃, and sintering time is 0.5～20h.
Described ZrO
2/ Y
2O
3The preparation method of composite target material is:
Adopt sol-gel method to prepare ZrO
2/ Y
2O
3Composite granule, Y in composite granule
2O
3Shared massfraction is 6%～20%, adds the PVA that accounts for its massfraction 5～10% and mix in composite granule, is pressed into living embryo sheet, and then 600 ℃ of insulation 90min binder removals, at 900～1600 ℃ of lower sintering 0.5～20h, thereby obtains required ZrO
2/ Y
2O
3Composite target material;
The calcium oxide-based ceramic core that adopts preparation method provided by the invention to obtain changes the hydration resistance of core by the mode at carbonate-free lime core blank surface plated film.With respect to ceramic base core of the prior art, expanded the starting material of core, can adopt carbonate-free lime to carry out the core preparation; Utilize the mode of nano thin-film at core blank surface plated film, plated film adopts ZrO
2/ Y
2O
3Composite target material has reached the aquation protection to the calcium oxide core, and more has been conducive to the core demoulding, is applicable to the core preparation in titanium alloy precision casting technique.
Description of drawings
Fig. 1 is the structural representation of the magnetic control sputtering device of technical solution of the present invention use
Embodiment
Below in conjunction with drawings and Examples, technical solution of the present invention is further described
Adopt technical solution of the present invention to prepare a kind of step of method of calcium oxide ceramics core as follows:
Step 1: take paraffin, 6kg beeswax and the 1.5kg oleic acid of 7.5kg, and mix and obtain softening agent, then take the 85kg calcium oxide powder, mix with the above-mentioned softening agent of preparation, then moulding, sintering obtains carbonate-free lime core blank;
Step 2: adopt sol-gel method to prepare ZrO
2/ Y
2O
3Composite granule adds the PVA(polyvinyl alcohol that accounts for its massfraction 5% in composite granule) and mix, be pressed into living embryo sheet, then at 600 ℃ of insulation 90min binder removals, at 900 ℃ of lower sintering 0.5h, thereby obtain required ZrO
2/ Y
2O
3Composite target material;
Step 3: with the calcium oxide-based ceramic core blank surface of sand papering, and with the cleaning of core blank, dry for standby;
Step 4: with ZrO
2/ Y
2O
3Calcium oxide core blank 4 after composite target material 3 and surface treatment is placed in respectively main sputtering chamber 1 and the Sample Room 2 of magnetic control sputtering device, main sputtering chamber 1 and Sample Room 2 is vacuumized, when vacuum tightness reaches 4 * 10-3Pa, to ZrO
2/ Y
2O
3Composite target material carries out pre-sputtering and removes its surface impurity, then rotates substrate rotating disk 5 and makes the calcium oxide core blank 4 on substrate rotating disk 5 be placed in aura, passes into argon gas to main sputtering chamber, and adjustable pressure to 4 * 10-1Pa regulates calcium oxide core blank 4 and ZrO
2/ Y
2O
3The spacing of composite target material 3 is regulated the sputter of sputtering power 200W build-up of luminance between 30mm, take out sample after sputter 0.1h;
Step 5: the surface is prepared ZrO
2/ Y
2O
3Film calcium oxide-based ceramic core later carries out intensified-sintered, and sintering temperature is that sintering temperature is 900 ℃, sintering time 0.5h.
It is that 98% climatic chamber carries out the aquation experiment that the above-mentioned calcium oxide-based ceramic core of water resistant type that is prepared into is placed in 26 ℃, humidity, hydration time is respectively 1,5,10,15,20 day, subsequently the coated powder ceramic plate after the aquation experiment is weighed, before and after contrast, the changes in weight of coated powder ceramic plate is shown in Table 1.
Table 1 aquation experimental result
| Time/ |
1 | 5 | 10 | 15 | 20 |
| Rate of body weight gain/% | 0.027 | 0.033 | 0.066 | 0.072 | 0.099 |
As seen from Table 1, after the calcium oxide-based ceramic core of water resistant type of preparing is tested through the aquation of 20 days, the weight rate of body weight gain is only 0.099%, has good water resistant effect, can satisfy the demand of titanium alloy precision casting.
Embodiment two:
The preparation of calcium oxide-based ceramic core, it is comprised of following steps:
Step 1: take paraffin, 0.5kg beeswax, the 0.5kg oleic acid of 4kg, and mix and obtain softening agent, then take the 95kg calcium oxide powder, mix with the above-mentioned softening agent of preparation, then moulding, sintering obtains carbonate-free lime core blank.
Step 2: adopt sol-gel method to prepare ZrO
2/ Y
2O
3Composite granule adds the PVA that accounts for its massfraction 10% and mixes in composite granule, be pressed into living embryo sheet, and then 600 ℃ of insulation 90min binder removals, at 1600 ℃ of lower sintering 20h, thereby obtains required target;
Step 3: with the calcium oxide-based ceramic core of sand papering surface, and with core cleaning, dry for standby;
Step 4: with ZrO
2/ Y
2O
3Calcium oxide core blank 4 after composite target material 3 and surface treatment is placed in respectively main sputtering chamber 1 and the Sample Room 2 of magnetic control sputtering device, main sputtering chamber 1 and Sample Room 2 is vacuumized, when vacuum tightness reaches 3 * 10-3Pa, to ZrO
2/ Y
2O
3Composite target material carries out pre-sputtering and removes its surface impurity, then rotates substrate rotating disk 5 and makes the calcium oxide core blank 4 on substrate rotating disk 5 be placed in aura, passes into argon gas to main sputtering chamber, and adjustable pressure to 3 * 10-1Pa regulates calcium oxide core blank 4 and ZrO
2/ Y
2O
3The spacing of composite target material 3 is regulated the sputter of sputtering power 400W build-up of luminance between 40mm, take out sample after sputter 1h;
Step 5: the surface is prepared ZrO
2/ Y
2O
3Film calcium oxide-based ceramic core later carries out intensified-sintered, and sintering temperature is 1600 ℃, sintering time 20h.
It is that 98% climatic chamber carries out the aquation experiment that the above-mentioned calcium oxide-based ceramic core of water resistant type that is prepared into is placed in 26 ℃, humidity, hydration time is respectively 1,5,10,15,20 day, subsequently the coated powder ceramic plate after the aquation experiment is weighed, before and after contrast, the changes in weight of coated powder ceramic plate is shown in Table 2.
Table 2 aquation experimental result
| Time/ |
1 | 5 | 10 | 15 | 20 |
| Rate of body weight gain/% | 0.015 | 0.023 | 0.032 | 0.039 | 0.043 |
As seen from Table 2, after the calcium oxide-based ceramic core of water resistant type of preparing is tested through the aquation of 20 days, the weight rate of body weight gain is only 0.043%, has good water resistant effect, can satisfy the demand of titanium alloy precision casting.
Embodiment three
The preparation of calcium oxide-based ceramic core, it is comprised of following steps:
Step 1: the paraffin, 3.5kg beeswax and the 0.5kg oleic acid that take 6kg mix, and mix and obtain softening agent, then take the 90kg calcium oxide powder, mix with the above-mentioned softening agent of preparation, and then moulding, sintering obtains carbonate-free lime core blank;
Step 2: adopt sol-gel method to prepare ZrO
2/ Y
2O
3Composite granule adds the PVA that accounts for its massfraction 8% and mixes in composite granule, be pressed into living embryo sheet, and then 600 ℃ of insulation 90min binder removals, at 1100 ℃ of lower sintering 5h, thereby obtains required target;
Step 3: with the calcium oxide-based ceramic core of sand papering surface, and with core cleaning, dry for standby;
Step 4: with ZrO
2/ Y
2O
3Calcium oxide core blank 4 after composite target material 3 and surface treatment is placed in respectively main sputtering chamber 1 and the Sample Room 2 of magnetic control sputtering device, main sputtering chamber 1 and Sample Room 2 is vacuumized, when vacuum tightness reaches 3 * 10-3Pa, to ZrO
2/ Y
2O
3Composite target material carries out pre-sputtering and removes its surface impurity, then rotates substrate rotating disk 5 and makes the calcium oxide core blank 4 on substrate rotating disk 5 be placed in aura, passes into argon gas to main sputtering chamber, and adjustable pressure to 2 * 10-1Pa regulates calcium oxide core blank 4 and ZrO
2/ Y
2O
3The spacing of composite target material 3 is regulated the sputter of sputtering power 250W build-up of luminance between 35mm, take out sample after sputter 0.5h;
Step 5: the surface is prepared ZrO
2/ Y
2O
3Film calcium oxide-based ceramic core later carries out intensified-sintered, and sintering temperature is 1300 ℃, sintering time 10h.
It is that 98% climatic chamber carries out the aquation experiment that the above-mentioned calcium oxide-based ceramic core of water resistant type that is prepared into is placed in 26 ℃, humidity, hydration time is respectively 1,5,10,15,20 day, subsequently the coated powder ceramic plate after the aquation experiment is weighed, before and after contrast, the changes in weight of coated powder ceramic plate is shown in Table 3.
Table 3 aquation experimental result
| Time/ |
1 | 5 | 10 | 15 | 20 |
| Rate of body weight gain/% | 0.029 | 0.032 | 0.044 | 0.049 | 0.077 |
As seen from Table 3, after the calcium oxide-based ceramic core of water resistant type of preparing is tested through the aquation of 20 days, the weight rate of body weight gain is only 0.077%, has good water resistant effect, can satisfy the demand of titanium alloy precision casting.
Embodiment four
The preparation of calcium oxide-based ceramic core, it is comprised of following steps:
Step 1: the paraffin, 1.7kg beeswax and the 0.8kg oleic acid that take 7.5kg mix, and mix and obtain softening agent, then take the 90kg calcium oxide powder, mix with the above-mentioned softening agent of preparation, and then moulding, sintering obtains carbonate-free lime core blank.
Step 2: adopt sol-gel method to prepare ZrO
2/ Y
2O
3Composite granule adds the PVA that accounts for its massfraction 8% and mixes in composite granule, be pressed into living embryo sheet, and then 600 ℃ of insulation 90min binder removals, at 1300 ℃ of lower sintering 15h, thereby obtains required target;
Step 3: with the calcium oxide-based ceramic core of sand papering surface, and with core cleaning, dry for standby;
Step 4: with ZrO
2/ Y
2O
3Calcium oxide core blank 4 after composite target material 3 and surface treatment is placed in respectively main sputtering chamber 1 and the Sample Room 2 of magnetic control sputtering device, main sputtering chamber 1 and Sample Room 2 is vacuumized, when vacuum tightness reaches 3 * 10-3Pa, to ZrO
2/ Y
2O
3Composite target material carries out pre-sputtering and removes its surface impurity, then rotates substrate rotating disk 5 and makes the calcium oxide core blank 4 on substrate rotating disk 5 be placed in aura, passes into argon gas to main sputtering chamber, and adjustable pressure to 1 * 10-1Pa regulates calcium oxide core blank 4 and ZrO
2/ Y
2O
3The spacing of composite target material 3 is regulated the sputter of sputtering power 300W build-up of luminance between 35mm, take out sample after sputter 0.7h;
Step 5: the surface is prepared ZrO
2/ Y
2O
3Film calcium oxide-based ceramic core later carries out intensified-sintered, and sintering temperature is 1400 ℃, sintering time 15h.
It is that 98% climatic chamber carries out the aquation experiment that the above-mentioned calcium oxide-based ceramic core of water resistant type that is prepared into is placed in 26 ℃, humidity, hydration time is respectively 1,5,10,15,20 day, subsequently the coated powder ceramic plate after the aquation experiment is weighed, before and after contrast, the changes in weight of coated powder ceramic plate is shown in Table 4.
Table 4 aquation experimental result
| Time/ |
1 | 5 | 10 | 15 | 20 |
| Rate of body weight gain/% | 0.027 | 0.033 | 0.048 | 0.052 | 0.065 |
As seen from Table 4, after the calcium oxide-based ceramic core of water resistant type of preparing is tested through the aquation of 20 days, the weight rate of body weight gain is only 0.065%, has good water resistant effect, can satisfy the demand of titanium alloy precision casting.
Claims (1)
1. the preparation method of a calcium oxide-based ceramic core, it is characterized in that: the step of the method is:
⑴ prepare calcium oxide core blank
Chemical composition and the weight percent of calcium oxide core blank are: calcium oxide powder 85～95wt%, softening agent 5～15wt%, the chemical composition of described softening agent and weight percent are: paraffin 50～80wt%, beeswax 10～40wt%, oleic acid are 5～10wt%;
Take in proportion paraffin, beeswax and oleic acid, mix, obtain softening agent, then take in proportion calcium oxide powder and softening agent, mix, press sintering after the shape requirement moulding of core, obtain calcium oxide core blank;
⑵ prepare ZrO in calcium oxide-based ceramic core blank surface
2/ Y
2O
3Film
At first use the calcium oxide-based ceramic core blank surface of sand papering, and with the cleaning of core blank, dry for standby, then with ZrO
2/ Y
2O
3Calcium oxide core blank (4) after composite target material (3) and surface treatment is placed in respectively main sputtering chamber (1) and the Sample Room (2) of magnetic control sputtering device, main sputtering chamber (1) and Sample Room (2) are vacuumized, when vacuum tightness reaches 4 * 10
-3Below Pa, to ZrO
2/ Y
2O
3Composite target material carries out pre-sputtering and removes its surface impurity, then rotates substrate rotating disk (5) and makes the calcium oxide core blank (4) on substrate rotating disk (5) be placed in aura, passes into argon gas to main sputtering chamber, adjustable pressure to 1 * 10
-1～4 * 10
-1Pa regulates calcium oxide core blank (4) and ZrO
2/ Y
2O
3The spacing of composite target material (3) is regulated sputtering power between 200～400W, build-up of luminance sputter, sputter 0.1～1h between 30～40mm.
(3) core is intensified-sintered
The surface is prepared ZrO
2/ Y
2O
3Film calcium oxide-based ceramic core later carries out intensified-sintered, and sintering temperature is 900～1600 ℃, and sintering time is 0.5～20h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103386703A (en) * | 2013-07-24 | 2013-11-13 | 中国南方航空工业(集团)有限公司 | Forming method for ceramic die core |
| CN103639396A (en) * | 2013-11-29 | 2014-03-19 | 沈阳化工大学 | Method for producing metallic titanium and titanium alloy castings through ceramic molds |
| CN103693976A (en) * | 2013-12-09 | 2014-04-02 | 中国航空工业集团公司北京航空材料研究院 | Method for preparing silicon oxide-based ceramic core for titanium and titanium alloy casting |
| CN104128556B (en) * | 2014-05-24 | 2016-04-13 | 芜湖浙鑫新能源有限公司 | The ceramic core that a kind of inorganic easy depoling is defeated and dispersed |
| CN105732007A (en) * | 2016-01-25 | 2016-07-06 | 西安交通大学 | Fast preparation method of calcium oxide based ceramic casting mold for manufacturing complex parts |
| CN106082997A (en) * | 2016-06-14 | 2016-11-09 | 西安交通大学 | A kind of method preparing calcium oxide-based ceramic-mould by chemical gaseous phase deposition approach |
| CN110937884A (en) * | 2019-12-05 | 2020-03-31 | 中国航发北京航空材料研究院 | Preparation method of titanium-based alloy powder hot isostatic pressing sheath inner cavity isolation layer |
| CN115382856A (en) * | 2022-10-25 | 2022-11-25 | 江苏容正医药科技有限公司 | Plasma ultra-clean processing method, system, device and medium |
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| 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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| CN103386703A (en) * | 2013-07-24 | 2013-11-13 | 中国南方航空工业(集团)有限公司 | Forming method for ceramic die core |
| CN103639396B (en) * | 2013-11-29 | 2017-01-04 | 沈阳化工大学 | Utilize the method that ceramic mould prepares Titanium and titanium alloy casting |
| CN103639396A (en) * | 2013-11-29 | 2014-03-19 | 沈阳化工大学 | Method for producing metallic titanium and titanium alloy castings through ceramic molds |
| CN103693976A (en) * | 2013-12-09 | 2014-04-02 | 中国航空工业集团公司北京航空材料研究院 | Method for preparing silicon oxide-based ceramic core for titanium and titanium alloy casting |
| CN104128556B (en) * | 2014-05-24 | 2016-04-13 | 芜湖浙鑫新能源有限公司 | The ceramic core that a kind of inorganic easy depoling is defeated and dispersed |
| CN105732007A (en) * | 2016-01-25 | 2016-07-06 | 西安交通大学 | Fast preparation method of calcium oxide based ceramic casting mold for manufacturing complex parts |
| CN105732007B (en) * | 2016-01-25 | 2019-01-15 | 西安交通大学 | A kind of calcium oxide-based ceramic-mould fast preparation method for complex parts manufacture |
| CN106082997A (en) * | 2016-06-14 | 2016-11-09 | 西安交通大学 | A kind of method preparing calcium oxide-based ceramic-mould by chemical gaseous phase deposition approach |
| CN106082997B (en) * | 2016-06-14 | 2018-06-26 | 西安交通大学 | A kind of method that calcium oxide-based ceramic-mould is prepared by chemical vapor deposition means |
| CN110937884A (en) * | 2019-12-05 | 2020-03-31 | 中国航发北京航空材料研究院 | Preparation method of titanium-based alloy powder hot isostatic pressing sheath inner cavity isolation layer |
| CN115382856A (en) * | 2022-10-25 | 2022-11-25 | 江苏容正医药科技有限公司 | Plasma ultra-clean processing method, system, device and medium |
| CN116274878A (en) * | 2023-03-03 | 2023-06-23 | 九牧厨卫股份有限公司 | Salt core material, salt core for titanium alloy casting and preparation method of salt core |
| CN116274878B (en) * | 2023-03-03 | 2024-07-30 | 九牧厨卫股份有限公司 | Salt core material, salt core for titanium alloy casting and preparation method of salt core |
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Application publication date: 20130619 |