CN103964855A - Coated zirconium boride based core and preparation method thereof - Google Patents
Coated zirconium boride based core and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a coated zirconium boride based core and a preparation method thereof. The coated zirconium boride based core comprises raw materials in percentage by weight as follows: 5-20 wt% of a mineralizer, 10-15 wt% of a plasticizer and the balance of rear earth coated boron nitride powder, wherein the mineralizer is one of CaO and MgO or composited by mixing CaO and MgO; and the plasticizer is prepared in percentage by mass as follows: 75-90 wt% of beewax, 5-20 wt% of paraffin wax and the balance of oleic acid. The prepared coated zirconium boride based core has excellent sintering character, good indoor high temperature mechanical properties and excellent chemical reactionlessness with titanium melt and decoring performance.
Description
technical field:
The present invention relates to precision casting field, specifically a kind of cladded type zirconium boride 99.5004323A8ure fundamental mode core and preparation method thereof.
background technology:
The complicated inner cavity of alloy-steel casting is mainly by carrying out moulding with prefabricated ceramic core, and after foundry goods is cast, manages to remove.Its technical process is as follows: Tao Xin prepares, contains wax-pattern preparation, shell processed, shell dewaxing and roasting, alloy casting, the depoling of Tao Xin.As everyone knows, along with the startup of China's development large aircraft project and various new work engine research and development program elements, body, structure and performance thereof to titanium alloy precision casting are had higher requirement.
At present, research aluminum oxide, silica-based ceramic core comparatively widely, because core material does not possess the chemical reaction inertia good to molten titanium alloy and depoling complex process is difficult to be applied to titanium alloy fine casting field.Because zirconium boride 99.5004323A8ure and molten titanium alloy at high temperature have higher chemical reaction inertia, and the good high-temperature creep resistance of tool, zirconium boride 99.5004323A8ure is a kind of aggregate that is well suited for being used as titanium alloy fine casting ceramic core.Cause in recent years related scientific research personnel's concern, as the Chinese invention patent application of publication number 200610028168.9 discloses a kind of preparation method of the zirconium boride ceramic shell for titanium or titanium alloy precision casting, in this invention, adopting zirconium boride 99.5004323A8ure powder and acetic acid zirconium thereof or silicon sol is that binding agent is made painting slip.Because the shape of titanium alloy becomes increasingly complex, present titanium alloy casting is often with complicated inner cavity, and this integrity that requires core to possess good high-temperature creep resistance and then guarantee shape in titanium alloy casting process is also had higher requirement to the performance that removes to core simultaneously.But zirconium boride 99.5004323A8ure stable chemical performance removes and has brought certain difficulty to be especially difficult to remove with mechanical means for complex-shaped core to core.In order to improve the depoling performance of core, calcium oxide core material also receives related scientific research personnel's concern, as the Chinese invention patent application of CN 102531648 A discloses a kind of Ti alloy casting calcium oxide matrix ceramic core and preparation method, due to comparatively complicated in titanium alloy precision casting technique, general all more than two weeks from be prepared into duration of pouring of alloy containing the wax-pattern of Tao Xin, core in use will contact with water-based paint.After the core chance water that above-mentioned patent is prepared, hydration reaction occurs 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:
In order to make up prior art problem, the object of this invention is to provide a kind of cladded type zirconium boride 99.5004323A8ure fundamental mode core and preparation method thereof, the cladded type zirconium boride 99.5004323A8ure base ceramic core that the present invention prepares possess good sintering character, chamber mechanical behavior under high temperature good, there is good chemical reaction inertia and there is good depoling performance with titanium melt.
Technical scheme of the present invention is as follows:
A kind of cladded type zirconium boride 99.5004323A8ure base ceramic core, is characterized in that: the raw material being made up of following weight per-cent is prepared from: mineralizer 5-20wt%, softening agent 10-15 wt%, surplus are the coated zirconium boride powder of rare earth.
Described cladded type zirconium boride 99.5004323A8ure base ceramic core, is characterized in that: described mineralizer is that a kind of in CaO, MgO or two kinds mix composition with any mass ratio.
Described cladded type zirconium boride 99.5004323A8ure base ceramic core, is characterized in that: described softening agent is the mixing of beeswax, paraffin, three kinds of materials of oleic acid, and its mixing quality proportioning is: beeswax 75-90wt%, paraffin 5-20wt%, surplus are oleic acid.
The preparation method of described cladded type zirconium boride 99.5004323A8ure base ceramic core, is characterized in that, comprises the steps:
Step 1, prepare the powder of the coated zirconium boride 99.5004323A8ure of rare earth oxide;
Step 2, by the powder of coated rare earth oxide zirconium boride 99.5004323A8ure, softening agent and mineralizer heating and obtain cladded type zirconium boride 99.5004323A8ure fundamental mode core material by stirring to be mixed;
Step 3, to core material carry out moulding, sintering obtains zirconium boride 99.5004323A8ure base ceramic core; Described sintering temperature is 1500～1900 DEG C, and the time is 0.5～20h.
The preparation method of cladded type zirconium boride 99.5004323A8ure base ceramic core, is characterized in that: the powder of preparing the coated zirconium boride 99.5004323A8ure of rare earth oxide described in step 1, specifically comprises the steps:
The first step, prepare zirconium boride 99.5004323A8ure suspension: nonionogenic tenside is joined in deionized water and forms the first mixing solutions, wherein in every 100ml deionized water, contain 1-10g nonionogenic tenside; Boronation zirconium powder is joined in the first mixing solutions, stir and prepare zirconium boride 99.5004323A8ure suspension; The add-on of boronation zirconium powder is to add 1～2mol in every 100ml deionized water;
Second step, prepare rare earth oxide precursor solution: inorganic zirconates and inorganic yttrium salts are mixed as rare earth oxide presoma using any ratio, take inorganic zirconates and inorganic yttrium salts and put into the container that fills deionized water and stir and heat and make precursor solution;
The 3rd step, rare earth oxide precursor solution is joined in zirconium boride 99.5004323A8ure suspension, stir and obtain the second mixing solutions; In the second described mixing solutions, rare earth oxide presoma is 1:10-45 with the ratio of the molar weight of boronation zirconium powder;
The 4th step, add pH value to 8～11 of adjusting solution in the second mixing solutions to obtain the 3rd mixing solutions ammoniacal liquor;
The 5th step, oven dry the 3rd mixing solutions obtain drying powder;
The 6th step, will dry powder and carry out sintering and obtain the powder of the coated zirconium boride 99.5004323A8ure of rare earth oxide; Described sintering, temperature is 1200-1600 DEG C, the time is 0.5～20h.
The preparation method of described cladded type zirconium boride 99.5004323A8ure base ceramic core, is characterized in that: described inorganic zirconates is zirconium chloride or zirconium nitrate.
The preparation method of described cladded type zirconium boride 99.5004323A8ure base ceramic core, is characterized in that: described inorganic yttrium salts is Yttrium trichloride or Yttrium trinitrate.
The preparation method of described cladded type zirconium boride 99.5004323A8ure base ceramic core, is characterized in that: described rare earth oxide precursor solution, its molar mass percentage concentration is 0.01～22mol/L.
Advantage of the present invention is:
The rare earth oxide Coated powder that utilization of the present invention is prepared is as core aggregate, and by adding a certain amount of mineralizer as calcium oxide, magnesium oxide, improve on the one hand the sintering character of zirconium boride 99.5004323A8ure, utilize on the other hand calcium oxide, magnesium oxide to meet water and be easy to form corresponding calcium hydroxide, magnesium hydroxide and then make core defeated and dispersed, thereby improve the depoling performance of core.
embodiment:
Cladded type zirconium boride 99.5004323A8ure base ceramic core, the raw material being made up of following weight per-cent is prepared from: mineralizer 5-20wt%, softening agent 10-15 wt%, surplus are the coated zirconium boride powder of rare earth;
Mineralizer is that a kind of in CaO, MgO or two kinds mix composition with any mass ratio;
Softening agent is beeswax, paraffin, oleic acid, and its quality proportioning is: beeswax 75-90wt%, paraffin 5-20wt%, surplus are oleic acid.
The preparation method of cladded type zirconium boride 99.5004323A8ure base ceramic core, specifically comprises the steps:
Step 1, prepare the powder of the coated zirconium boride 99.5004323A8ure of rare earth oxide;
Step 2, by the powder of coated rare earth oxide zirconium boride 99.5004323A8ure, softening agent and mineralizer heating and obtain cladded type zirconium boride 99.5004323A8ure fundamental mode core material by stirring to be mixed;
Step 3, to core material carry out moulding, sintering obtains zirconium boride 99.5004323A8ure base ceramic core; Described sintering temperature is 1500～1900 DEG C, and the time is 0.5～20h.
Step 1 specifically comprises the steps:
The first step, prepare zirconium boride 99.5004323A8ure suspension: nonionogenic tenside is joined in deionized water and forms the first mixing solutions, wherein in every 100ml deionized water, contain 1-10g nonionogenic tenside; Boronation zirconium powder is joined in the first mixing solutions, stir and prepare zirconium boride 99.5004323A8ure suspension; The add-on of boronation zirconium powder is to add 1-2mol in every 100ml deionized water;
Second step, prepare rare earth oxide precursor solution: inorganic zirconates and inorganic yttrium salts are mixed as rare earth oxide presoma using any ratio, take inorganic zirconates and inorganic yttrium salts and put into the container that fills deionized water and stir and heat and make precursor solution;
The 3rd step, rare earth oxide precursor solution is joined in zirconium boride 99.5004323A8ure suspension, stir and obtain the second mixing solutions; The second described mixing solutions, its middle rare earth presoma is 1:10-45 with the ratio of the molar weight of boronation zirconium powder;
The 4th step, add pH value to 8～11 of adjusting solution in the second mixing solutions to obtain the 3rd mixing solutions ammoniacal liquor;
The 5th step, oven dry the 3rd mixing solutions obtain drying powder;
The 6th step, will dry powder and carry out sintering and obtain the powder of the coated zirconium boride 99.5004323A8ure of rare earth oxide; The temperature of sintering is 1200-1600 DEG C, and the time is 0.5～20h.
Inorganic zirconates is zirconium chloride or zirconium nitrate.
Inorganic yttrium salts is Yttrium trichloride or Yttrium trinitrate.
Rare earth oxide precursor solution, its molar mass percentage concentration is 0.01～22mol/L.
Further illustrate the present invention below by specific embodiment, just illustrate unrestrictedly, the improvement that those skilled in the art does under the inspiration of inventive concept, all drops in protection scope of the present invention.
Embodiment 1: the preparation of cladded type zirconium boride 99.5004323A8ure base ceramic core, comprises the following steps:
Step 1: prepare zirconium boride 99.5004323A8ure suspension: 1g Polyethylene Glycol-600 is joined in the deionized water of 100ml, the zirconium boride powder of 1mol is placed in to above-mentioned solution, and utilize ultrasonic wave to disperse to make zirconium boride 99.5004323A8ure suspension after 10min; The granularity of described zirconium boride powder is 100-500 order;
Step 2, prepare rare earth oxide presoma: the zirconium chloride taking is put into beaker and add the deionized water of 50ml, then put it in water-bath, water-bath temperature is 80 DEG C, utilizes magnetic stirrer 10h to prepare rare earth oxide precursor solution;
Step 3: utilize drop-burette that rare earth oxide precursor solution is added drop-wise in zirconium boride 99.5004323A8ure suspension, wherein rate of addition Φ >=1ml/min, and the mode of utilizing ultrasonic wave and mechanical stirring to combine mixes two kinds of solution, zirconium chloride with the ratio of the amount of substance of zirconium boride powder is: 1:43;
Step 4: ammoniacal liquor is passed into above-mentioned mixing solutions and makes the pH value of solution 8;
Step 5: dry at the temperature of 80 DEG C, time 10-24h, obtains drying powder;
Step 6: will dry powder and put into High Temperature Furnaces Heating Apparatus and carry out sintering and finally obtain the powder of the coated zirconium boride 99.5004323A8ure of rare earth oxide; The sintering temperature of described oven dry powder is 1200 DEG C, and sintering time is 0.5h;
Step 7: the powder of the coated zirconium boride 99.5004323A8ure of 5g calcium oxide, 6g beeswax, 1g paraffin, 3g oleic acid, 85g rare earth oxide is placed in to beaker, and utilizes water-bath that core material is heated to 70 DEG C and utilize magnetic stirring apparatus to mix;
Step 8: the core material mixing is put in core injector, suppressed core, wherein die temperature is 70 DEG C, and injection pressure is 10MPa, and the dwell time is 10s;
Step 9: the Zirconium powder of raw core for preparing embryo being put into lower saggar and imbedding stabilization treatment carries out sintering, and wherein heat-up rate is 2 DEG C/min, and sintering temperature is 1500 DEG C, and sintering time is 5h.
Embodiment 2:
The preparation of cladded type zirconium boride 99.5004323A8ure base ceramic core, comprises the following steps:
Step 1: prepare zirconium boride 99.5004323A8ure suspension: 10g polyoxyethylene glycol 800 is joined in the deionized water of 150ml, the zirconium boride powder of 3mol is placed in to above-mentioned solution, and utilize ultrasonic wave to disperse to make zirconium boride 99.5004323A8ure suspension after 60min; The granularity of described zirconium boride powder is 100-500 order;
Step 2, prepare rare earth oxide presoma: the Yttrium trichloride taking is put into beaker and add the dehydrated alcohol of 50ml, then put it in water-bath, water-bath temperature is 60 DEG C, utilizes magnetic stirrer 10h to prepare rare earth oxide precursor solution;
Step 3: utilize drop-burette that rare earth oxide precursor solution is added drop-wise in zirconium boride 99.5004323A8ure suspension, wherein rate of addition Φ >=1ml/min, and the mode of utilizing ultrasonic wave and mechanical stirring to combine mixes two kinds of solution, wherein Yttrium trichloride with the ratio of the amount of substance of zirconium boride powder is: 1:12;
Step 4: ammoniacal liquor is passed into above-mentioned mixing solutions and makes the pH value of solution 11;
Step 5: dry at the temperature of 150 DEG C, time 24h, obtains drying powder;
Step 6: will dry powder and put into High Temperature Furnaces Heating Apparatus and carry out sintering and finally obtain the powder of the coated zirconium boride 99.5004323A8ure of rare earth oxide; The sintering temperature of described oven dry powder is 1600 DEG C, and sintering time is 5h;
Step 7: coated to 20g magnesium oxide, 13.5g beeswax, 1.5g paraffin, 65g rare earth zirconium boride powder is placed in to beaker, and utilizes water-bath that core material is heated to 110 DEG C and utilize magnetic stirring apparatus to mix;
Step 8: the core material mixing is put in core injector, suppressed core, wherein die temperature is 110 DEG C, and injection pressure is 25MPa, and the dwell time is 30s;
Step 9: the Zirconium powder of raw core for preparing embryo being put into lower saggar and imbedding stabilization treatment carries out sintering, and wherein heat-up rate is 10 DEG C/min, and sintering temperature is 1900 DEG C, and sintering time is 3h.
Embodiment 3:
The preparation of cladded type zirconium boride 99.5004323A8ure base ceramic core, comprises the following steps:
Step 1: prepare zirconium boride 99.5004323A8ure suspension: 8g polyoxyethylene glycol 800 is joined in the deionized water of 130ml, the zirconium boride powder of 2mol is placed in to above-mentioned solution, and utilize ultrasonic wave to disperse to make zirconium boride 99.5004323A8ure suspension after 50min; The granularity of described zirconium boride powder is 100-500 order;
Step 2, prepare rare earth oxide presoma: 0.04mol zirconium nitrate, 0.06mol Yttrium trinitrate are put into beaker and add the deionized water of 130ml, then put it in water-bath, water-bath temperature is 90 DEG C, utilizes magnetic stirrer 10h to prepare rare earth oxide precursor solution;
Step 3: utilize drop-burette that rare earth oxide precursor solution is added drop-wise in zirconium boride 99.5004323A8ure suspension, wherein rate of addition Φ >=1ml/min, and the mode of utilizing ultrasonic wave and mechanical stirring to combine mixes two kinds of solution, its middle rare earth with the ratio of the amount of substance of zirconium boride powder is: 1:20;
Step 4: ammoniacal liquor is passed into above-mentioned mixing solutions and makes the pH value of solution 10;
Step 5: dry at the temperature of 130 DEG C, time 13h, obtains drying powder;
Step 6: will dry powder and put into High Temperature Furnaces Heating Apparatus and carry out sintering and finally obtain the powder of the coated zirconium boride 99.5004323A8ure of rare earth oxide; The sintering temperature of described oven dry powder is 1400 DEG C, and sintering time is 4h;
Step 7: coated to 4g calcium oxide, 11g magnesium oxide, 9.1g beeswax, 2.6g paraffin, 1.3g oleic acid, 72g rare earth oxide zirconium boride powder is placed in to beaker, and utilizes water-bath that core material is heated to 100 DEG C and utilize magnetic stirring apparatus to mix;
Step 8: the core material mixing is put in core injector, suppressed core, wherein die temperature is 100 DEG C, and injection pressure is 21MPa, and the dwell time is 20s;
Step 9: the Zirconium powder of raw core for preparing embryo being put into lower saggar and imbedding stabilization treatment carries out sintering, and wherein heat-up rate is 7 DEG C/min, and sintering temperature is 1600 DEG C, and sintering time is 3.5h.
Embodiment 4:
The preparation of cladded type zirconium boride 99.5004323A8ure base ceramic core, comprises the following steps:
Step 1: prepare zirconium boride 99.5004323A8ure suspension: 6g polyoxyethylene glycol 800 is joined in the deionized water of 120ml, the zirconium boride powder of 2mol is placed in to above-mentioned solution, and utilize ultrasonic wave to disperse to make zirconium boride 99.5004323A8ure suspension after 50min; The granularity of zirconium boride powder is 100-500 order;
Step 2, prepare rare earth oxide presoma: 0.027mol zirconium chloride, 0.03mol Yttrium trinitrate are put into beaker and add the deionized water of 130ml, then put it in water-bath, water-bath temperature is 90 DEG C, utilizes magnetic stirrer 10h to prepare rare earth oxide precursor solution;
Step 3: utilize drop-burette that rare earth oxide precursor solution is added drop-wise in zirconium boride 99.5004323A8ure suspension, wherein rate of addition Φ >=1ml/min, and the mode of utilizing ultrasonic wave and mechanical stirring to combine mixes two kinds of solution, its middle rare earth with the ratio of the amount of substance of zirconium boride powder is: 1:35;
Step 4: ammoniacal liquor is passed into above-mentioned mixing solutions and makes the pH value of solution 10;
Step 5: dry at the temperature of 115 DEG C, time 10h, obtains drying powder;
Step 6: will dry powder and put into High Temperature Furnaces Heating Apparatus and carry out sintering and finally obtain the powder of the coated zirconium boride 99.5004323A8ure of rare earth oxide; The sintering temperature of described oven dry powder is 1500 DEG C, and sintering time is 2h.
Step 7: coated to 11g calcium oxide, 4g magnesium oxide, 7.1g beeswax, 4.6g paraffin, 1.3g oleic acid, 72g rare earth oxide zirconium boride powder is placed in to beaker, and utilizes water-bath that core material is heated to 100 DEG C and utilize magnetic stirring apparatus to mix;
Step 8: the core material mixing is put in core injector, suppressed core, wherein die temperature is 95 DEG C, and injection pressure is 18MPa, and the dwell time is 14s;
Step 9: the Zirconium powder of raw core for preparing embryo being put into lower saggar and imbedding stabilization treatment carries out sintering, and wherein heat-up rate is 4 DEG C/min, and sintering temperature is 1650 DEG C, and sintering time is 2.5h.
Claims (8)
1. a cladded type zirconium boride 99.5004323A8ure base ceramic core, is characterized in that: the raw material being made up of following weight per-cent is prepared from: mineralizer 5-20wt%, softening agent 10-15 wt%, surplus are the coated zirconium boride powder of rare earth.
2. cladded type zirconium boride 99.5004323A8ure base ceramic core according to claim 1, is characterized in that: described mineralizer is that a kind of in CaO, MgO or two kinds mix composition with any mass ratio.
3. cladded type zirconium boride 99.5004323A8ure base ceramic core according to claim 1, it is characterized in that: described softening agent is the mixing of beeswax, paraffin, three kinds of materials of oleic acid, and its mixing quality proportioning is: beeswax 75-90wt%, paraffin 5-20wt%, surplus are oleic acid.
4. a preparation method for cladded type zirconium boride 99.5004323A8ure base ceramic core claimed in claim 1, is characterized in that, comprises the steps:
Step 1, prepare the powder of the coated zirconium boride 99.5004323A8ure of rare earth oxide;
Step 2, by the powder of coated rare earth oxide zirconium boride 99.5004323A8ure, softening agent and mineralizer heating and obtain cladded type zirconium boride 99.5004323A8ure fundamental mode core material by stirring to be mixed;
Step 3, to core material carry out moulding, sintering obtains zirconium boride 99.5004323A8ure base ceramic core; Described sintering temperature is 1500～1900 DEG C, and the time is 0.5～20h.
5. according to the preparation method of claim 4 cladded type zirconium boride 99.5004323A8ure base ceramic core, it is characterized in that: the powder of preparing the coated zirconium boride 99.5004323A8ure of rare earth oxide described in step 1, specifically comprises the steps:
The first step, prepare zirconium boride 99.5004323A8ure suspension: nonionogenic tenside is joined in deionized water and forms the first mixing solutions, wherein in every 100ml deionized water, contain 1-10g nonionogenic tenside; Boronation zirconium powder is joined in the first mixing solutions, stir and prepare zirconium boride 99.5004323A8ure suspension; The add-on of boronation zirconium powder is to add 1～2mol in every 100ml deionized water;
Second step, prepare rare earth oxide precursor solution: inorganic zirconates and inorganic yttrium salts are mixed as rare earth oxide presoma using any ratio, take inorganic zirconates and inorganic yttrium salts and put into the container that fills deionized water and stir and heat and make precursor solution;
The 3rd step, rare earth oxide precursor solution is joined in zirconium boride 99.5004323A8ure suspension, stir and obtain the second mixing solutions; In the second described mixing solutions, rare earth oxide presoma is 1:10-45 with the ratio of the molar weight of boronation zirconium powder;
The 4th step, add pH value to 8～11 of adjusting solution in the second mixing solutions to obtain the 3rd mixing solutions ammoniacal liquor;
The 5th step, oven dry the 3rd mixing solutions obtain drying powder;
The 6th step, will dry powder and carry out sintering and obtain the powder of the coated zirconium boride 99.5004323A8ure of rare earth oxide; Described sintering, temperature is 1200-1600 DEG C, the time is 0.5～20h.
6. the preparation method of cladded type zirconium boride 99.5004323A8ure base ceramic core according to claim 4, is characterized in that: described inorganic zirconates is zirconium chloride or zirconium nitrate.
7. the preparation method of cladded type zirconium boride 99.5004323A8ure base ceramic core according to claim 4, is characterized in that: described inorganic yttrium salts is Yttrium trichloride or Yttrium trinitrate.
8. according to the preparation method of the cladded type zirconium boride 99.5004323A8ure base ceramic core described in claim 4, it is characterized in that: described rare earth oxide precursor solution, its molar mass percentage concentration is 0.01～22mol/L.
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| CN116063081A (en) * | 2023-02-16 | 2023-05-05 | 西北工业大学 | ZrO synthesis by sol-gel method 2 Coated ZrB 2 Preparation method of particle composite powder |
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Application publication date: 20140806 |