CN103964851B - A kind of titanium alloy precision casting cladded type boron carbide base ceramic core and preparation method thereof - Google Patents
A kind of titanium alloy precision casting cladded type boron carbide base ceramic core and preparation method thereof Download PDFInfo
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- 229910052580 B4C Inorganic materials 0.000 title claims abstract description 104
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 42
- 239000000919 ceramic Substances 0.000 title claims abstract description 38
- 238000005495 investment casting Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 64
- 238000005245 sintering Methods 0.000 claims abstract description 35
- 235000013871 bee wax Nutrition 0.000 claims abstract description 11
- 239000012166 beeswax Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000012188 paraffin wax Substances 0.000 claims abstract description 11
- 239000004014 plasticizer Substances 0.000 claims abstract description 11
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 10
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000005642 Oleic acid Substances 0.000 claims abstract description 10
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000011162 core material Substances 0.000 claims description 71
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 45
- 239000000243 solution Substances 0.000 claims description 34
- 239000011259 mixed solution Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000000725 suspension Substances 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 239000002243 precursor Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 12
- 150000003746 yttrium Chemical class 0.000 claims description 9
- 150000003754 zirconium Chemical class 0.000 claims description 9
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 6
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 6
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 5
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 7
- 150000002910 rare earth metals Chemical class 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 3
- 239000010936 titanium Substances 0.000 abstract description 3
- 229910052719 titanium Inorganic materials 0.000 abstract description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 14
- 239000000292 calcium oxide Substances 0.000 description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 8
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical group [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 7
- 238000005266 casting Methods 0.000 description 7
- 239000000395 magnesium oxide Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 210000001161 mammalian embryo Anatomy 0.000 description 4
- 230000006641 stabilisation Effects 0.000 description 4
- 238000011105 stabilization Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229920002593 Polyethylene Glycol 800 Polymers 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229940085675 polyethylene glycol 800 Drugs 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- BNUDRLITYNMTPD-UHFFFAOYSA-N acetic acid;zirconium Chemical compound [Zr].CC(O)=O BNUDRLITYNMTPD-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229960003511 macrogol Drugs 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
Abstract
The invention discloses a kind of titanium alloy precision casting cladded type boron carbide base ceramic core and preparation method thereof, the raw material that titanium alloy precision casting cladded type boron carbide base ceramic core is made up of following weight percentage is prepared from: mineralizer 5-20wt%, plasticizer 10-15wt%, surplus are the coated boron carbide powder of rare earth.Wherein mineralizer is one in CaO, MgO or two kinds of mixing compositions, and the quality proportioning of plasticizer is: beeswax 75-90wt%, paraffin 5-20wt%, surplus are oleic acid.The titanium alloy precision casting cladded type boron carbide base ceramic core that the present invention prepares possess excellent sintering character, room mechanical behavior under high temperature good, there is good chemical reaction inertia with titanium melt and there is good depoling performance.
Description
technical field:
The present invention relates to hot investment casting field, specifically a kind of titanium alloy precision casting cladded type boron carbide base ceramic core and preparation method thereof.
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 technological 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 aluminium oxide, silica 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.Because boron carbide and molten titanium alloy at high temperature have higher chemical reaction inertia, and the high-temperature creep resistance that tool is good, boron carbide 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 boron carbide ceramics shell for titanium or titanium alloy hot investment casting, adopts boron carbide powder and acetic acid zirconium or Ludox 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 integrality of shape is also had higher requirement to the performance that removes of core simultaneously.But boron carbide 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, calcium oxide core material also receives the concern of related scientific research personnel, Chinese invention patent application as CN102531648A 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, 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:
In order to make up prior art problem, the object of this invention is to provide a kind of titanium alloy precision casting cladded type boron carbide base ceramic core and preparation method thereof, the titanium alloy precision casting cladded type boron carbide base ceramic core that the present invention prepares possesses excellent sintering character, room mechanical behavior under high temperature well, with titanium melt has good chemical reaction inertia, and has good depoling performance.
Technical scheme of the present invention is as follows:
A kind of titanium alloy precision casting cladded type boron carbide base ceramic core, is characterized in that: the raw material be made up of following weight percentage is prepared from: mineralizer 5-20wt%, plasticizer 10-15wt%, surplus are the coated boron carbide powder of rare earth.
Described titanium alloy precision casting cladded type boron carbide base ceramic core, is characterized in that: described mineralizer is that one in CaO, MgO or two kinds are with any mass ratio mixing composition.
Described titanium alloy precision casting cladded type boron carbide base ceramic core, it is characterized in that: described plasticizer is the mixing of beeswax, paraffin, oleic acid three kinds of materials, and its mixing quality proportioning is: beeswax 75-90wt%, paraffin 5-20wt%, surplus are oleic acid.
The preparation method of described titanium alloy precision casting cladded type boron carbide base ceramic core, is characterized in that, comprise the steps:
The powder of step one, preparation rare earth oxide clad boron carbide;
Step 2, the powder of rare earth oxide clad boron carbide, plasticizer and mineralizer heated and passes through to stir to be mixed to obtain titanium alloy precision casting cladded type boron carbide base ceramic core material;
Step 3, core material carried out to moulding, sintering obtains boron carbide base ceramic core; Described sintering temperature is 1500 ~ 1900 DEG C, and the time is 0.5 ~ 20h.
The titanium alloy precision casting preparation method of cladded type boron carbide base ceramic core, is characterized in that: the powder of the preparation rare earth oxide clad boron carbide described in step one, specifically comprises the steps:
The first step, prepare boron carbide suspension: joined by non-ionic surface active agent in deionized water and form the first mixed solution, wherein in every 100ml deionized water containing 1-10g non-ionic surface active agent; Boron carbide powder is joined in the first mixed solution, stir and prepare boron carbide suspension; The addition of boron carbide powder adds 1 ~ 2mol in every 100ml deionized water;
Second step, prepare rare earth oxide precursor solution: 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;
3rd step, rare earth oxide precursor solution is joined in boron carbide suspension, stir and obtain the second mixed solution; In the second described mixed solution, rare earth oxide presoma is 1:10-45 with the ratio of the mole of boron carbide powder;
4th step, ammoniacal liquor is added pH value to 8 ~ 11 adjusting solution in the second mixed solution obtain the 3rd mixed solution;
5th step, oven dry the 3rd mixed solution obtain drying powder;
6th step, by oven dry powder carry out sintering the powder obtaining rare earth oxide clad boron carbide; Described sintering, temperature is 1200-1600 DEG C, and the time is 0.5 ~ 20h.
The preparation method of described titanium alloy precision casting cladded type boron carbide base ceramic core, is characterized in that: described inorganic zirconium salts is zirconium chloride or zirconium nitrate.
The preparation method of described titanium alloy precision casting cladded type boron carbide base ceramic core, is characterized in that: described inorganic yttrium salts is yttrium chloride or yttrium nitrate.
The preparation method of described titanium alloy precision casting cladded type boron carbide base ceramic core, is characterized in that: described rare earth oxide precursor solution, its molal weight percent concentration is 0.01 ~ 22mol/L.
Advantage of the present invention is:
The present invention utilizes the rare earth oxide clad type powder prepared as core aggregate, and by adding a certain amount of mineralizer as calcium oxide, magnesia, improve the sintering character of boron carbide on the one hand, utilize calcium oxide, magnesia to meet water to be on the other hand easy to form corresponding calcium hydroxide, magnesium hydroxide and then make core defeated and dispersed, thus improve the depoling performance of core.
detailed description of the invention:
Titanium alloy precision casting cladded type boron carbide base ceramic core, the raw material be made up of following weight percentage is prepared from: mineralizer 5-20wt%, plasticizer 10-15wt%, surplus are the coated boron carbide powder of rare earth;
Mineralizer is that one in CaO, MgO or two kinds are with any mass ratio mixing composition;
Plasticizer is beeswax, paraffin, oleic acid, and its quality proportioning is: beeswax 75-90wt%, paraffin 5-20wt%, surplus are oleic acid.
The titanium alloy precision casting preparation method of cladded type boron carbide base ceramic core, specifically comprises the steps:
The powder of step one, preparation rare earth oxide clad boron carbide;
Step 2, the powder of rare earth oxide clad boron carbide, plasticizer and mineralizer heated and passes through to stir to be mixed to obtain titanium alloy precision casting cladded type boron carbide base ceramic core material;
Step 3, core material carried out to moulding, sintering obtains boron carbide base ceramic core; Described sintering temperature is 1500 ~ 1900 DEG C, and the time is 0.5 ~ 20h.
Step one specifically comprises the steps:
The first step, prepare boron carbide suspension: joined by non-ionic surface active agent in deionized water and form the first mixed solution, wherein in every 100ml deionized water containing 1-10g non-ionic surface active agent; Boron carbide powder is joined in the first mixed solution, stir and prepare boron carbide suspension; The addition of boron carbide powder adds 1-2mol in every 100ml deionized water;
Second step, prepare rare earth oxide precursor solution: 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;
3rd step, rare earth oxide precursor solution is joined in boron carbide suspension, stir and obtain the second mixed solution; The second described mixed solution, its middle rare earth presoma is 1:10-45 with the ratio of the mole of boron carbide powder;
4th step, ammoniacal liquor is added pH value to 8 ~ 11 adjusting solution in the second mixed solution obtain the 3rd mixed solution;
5th step, oven dry the 3rd mixed solution obtain drying powder;
6th step, by oven dry powder carry out sintering the powder obtaining rare earth oxide clad boron carbide; The temperature of sintering is 1200-1600 DEG C, and the time is 0.5 ~ 20h.
Inorganic zirconium salts is zirconium chloride or zirconium nitrate.
Inorganic yttrium salts is yttrium chloride or yttrium nitrate.
Rare earth oxide precursor solution, its molal weight percent concentration is 0.01 ~ 22mol/L.
Further illustrate the present invention below by specific embodiment, just illustrate unrestricted, the improvement that those skilled in the art does under the inspiration of inventive concept, all drop in protection scope of the present invention.
Embodiment 1: the titanium alloy precision casting preparation of cladded type boron carbide base ceramic core, comprises the following steps:
Step one: prepare boron carbide suspension: join in the deionized water of 100ml by 1g Macrogol 600, is placed in above-mentioned solution by the boron carbide powder of 1mol, and makes boron carbide suspension after utilizing ultrasonic wave to disperse 10min; The granularity of described boron carbide powder is 100-500 order;
Step 2, prepare rare earth oxide presoma: the zirconium chloride taken is put into beaker and adds 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 buret to be added drop-wise in boron carbide suspension by rare earth oxide precursor solution, wherein rate of addition Φ >=1ml/min, and the mode utilizing ultrasonic wave and mechanical agitation to combine makes two kinds of solution mix, zirconium chloride with the ratio of the amount of substance of boron carbide powder is: 1:43;
Step 4: ammoniacal liquor is passed into above-mentioned mixed solution 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: oven dry powder is put into high temperature furnace and carries out sintering the powder finally obtaining rare earth oxide clad boron carbide; The sintering temperature of described oven dry powder is 1200 DEG C, and sintering time is 0.5h;
Step 7: the powder of 5g calcium oxide, 6g beeswax, 1g paraffin, 3g oleic acid, 85g rare earth oxide clad boron carbide is placed in beaker, and utilize water-bath core material is heated to 70 DEG C and utilizes magnetic stirring apparatus to mix;
Step 8: the core material mixed is put in core injector, carry out compacting core, wherein mold temperature is 70 DEG C, and injection pressure is 10MPa, and the dwell time is 10s;
Step 9: raw for the core prepared embryo is put into lower saggar and the Zirconium powder imbedding stabilization processes sinters, wherein programming rate is 2 DEG C/min, and sintering temperature is 1500 DEG C, and sintering time is 5h.
Embodiment 2:
The titanium alloy precision casting preparation of cladded type boron carbide base ceramic core, comprises the following steps:
Step one: prepare boron carbide suspension: join in the deionized water of 150ml by 10g polyethylene glycol-800, is placed in above-mentioned solution by the boron carbide powder of 3mol, and makes boron carbide suspension after utilizing ultrasonic wave to disperse 60min; The granularity of described boron carbide powder is 100-500 order;
Step 2, prepare rare earth oxide presoma: the yttrium chloride taken is put into beaker and adds the absolute ethyl 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 buret to be added drop-wise in boron carbide suspension by rare earth oxide precursor solution, wherein rate of addition Φ >=1ml/min, and the mode utilizing ultrasonic wave and mechanical agitation to combine makes two kinds of solution mix, wherein yttrium chloride with the ratio of the amount of substance of boron carbide powder is: 1:12;
Step 4: ammoniacal liquor is passed into above-mentioned mixed solution 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: oven dry powder is put into high temperature furnace and carries out sintering the powder finally obtaining rare earth oxide clad boron carbide; The sintering temperature of described oven dry powder is 1600 DEG C, and sintering time is 5h;
Step 7: 20g magnesia, 13.5g beeswax, 1.5g paraffin, the coated boron carbide powder of 65g rare earth are placed in beaker, and utilize water-bath core material is heated to 110 DEG C and utilizes magnetic stirring apparatus to mix;
Step 8: the core material mixed is put in core injector, carry out compacting core, wherein mold temperature is 110 DEG C, and injection pressure is 25MPa, and the dwell time is 30s;
Step 9: raw for the core prepared embryo is put into lower saggar and the Zirconium powder imbedding stabilization processes sinters, wherein programming rate is 10 DEG C/min, and sintering temperature is 1900 DEG C, and sintering time is 3h.
Embodiment 3:
The titanium alloy precision casting preparation of cladded type boron carbide base ceramic core, comprises the following steps:
Step one: prepare boron carbide suspension: join in the deionized water of 130ml by 8g polyethylene glycol-800, is placed in above-mentioned solution by the boron carbide powder of 2mol, and makes boron carbide suspension after utilizing ultrasonic wave to disperse 50min; The granularity of described boron carbide powder is 100-500 order;
Step 2, prepare rare earth oxide presoma: 0.04mol zirconium nitrate, 0.06mol yttrium nitrate are put into beaker and added 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 buret to be added drop-wise in boron carbide suspension by rare earth oxide precursor solution, wherein rate of addition Φ >=1ml/min, and the mode utilizing ultrasonic wave and mechanical agitation to combine makes two kinds of solution mix, its middle rare earth with the ratio of the amount of substance of boron carbide powder is: 1:20;
Step 4: ammoniacal liquor is passed into above-mentioned mixed solution 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: oven dry powder is put into high temperature furnace and carries out sintering the powder finally obtaining rare earth oxide clad boron carbide; The sintering temperature of described oven dry powder is 1400 DEG C, and sintering time is 4h;
Step 7: 4g calcium oxide, 11g magnesia, 9.1g beeswax, 2.6g paraffin, 1.3g oleic acid, 72g rare earth oxide clad boron carbide powder are placed in beaker, and utilize water-bath core material is heated to 100 DEG C and utilizes magnetic stirring apparatus to mix;
Step 8: the core material mixed is put in core injector, carry out compacting core, wherein mold temperature is 100 DEG C, and injection pressure is 21MPa, and the dwell time is 20s;
Step 9: raw for the core prepared embryo is put into lower saggar and the Zirconium powder imbedding stabilization processes sinters, wherein programming rate is 7 DEG C/min, and sintering temperature is 1600 DEG C, and sintering time is 3.5h.
Embodiment 4:
The titanium alloy precision casting preparation of cladded type boron carbide base ceramic core, comprises the following steps:
Step one: prepare boron carbide suspension: join in the deionized water of 120ml by 6g polyethylene glycol-800, is placed in above-mentioned solution by the boron carbide powder of 2mol, and makes boron carbide suspension after utilizing ultrasonic wave to disperse 50min; The granularity of boron carbide powder is 100-500 order;
Step 2, prepare rare earth oxide presoma: 0.027mol zirconium chloride, 0.03mol yttrium nitrate are put into beaker and added 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 buret to be added drop-wise in boron carbide suspension by rare earth oxide precursor solution, wherein rate of addition Φ >=1ml/min, and the mode utilizing ultrasonic wave and mechanical agitation to combine makes two kinds of solution mix, its middle rare earth with the ratio of the amount of substance of boron carbide powder is: 1:35;
Step 4: ammoniacal liquor is passed into above-mentioned mixed solution 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: oven dry powder is put into high temperature furnace and carries out sintering the powder finally obtaining rare earth oxide clad boron carbide; The sintering temperature of described oven dry powder is 1500 DEG C, and sintering time is 2h.
Step 7: 11g calcium oxide, 4g magnesia, 7.1g beeswax, 4.6g paraffin, 1.3g oleic acid, 72g rare earth oxide clad boron carbide powder are placed in beaker, and utilize water-bath core material is heated to 100 DEG C and utilizes magnetic stirring apparatus to mix;
Step 8: the core material mixed is put in core injector, carry out compacting core, wherein mold temperature is 95 DEG C, and injection pressure is 18MPa, and the dwell time is 14s;
Step 9: raw for the core prepared embryo is put into lower saggar and the Zirconium powder imbedding stabilization processes sinters, wherein programming rate is 4 DEG C/min, and sintering temperature is 1650 DEG C, and sintering time is 2.5h.
Claims (5)
1. a titanium alloy precision casting cladded type boron carbide base ceramic core, is characterized in that: the raw material be made up of following weight percentage is prepared from: mineralizer 5-20wt%, plasticizer 10-15wt%, surplus are the powder of rare earth oxide clad boron carbide; Described mineralizer is that one in CaO, MgO or two kinds are with any mass ratio mixing composition; Described plasticizer is the mixing of beeswax, paraffin, oleic acid three kinds of materials, and its mixing quality proportioning is: beeswax 75-90wt%, paraffin 5-20wt%, surplus are oleic acid.
2. a preparation method for titanium alloy precision casting cladded type boron carbide base ceramic core according to claim 1, is characterized in that, comprises the steps: the powder of step one, preparation rare earth oxide clad boron carbide; Step 2, the powder of rare earth oxide clad boron carbide, plasticizer and mineralizer heated and passes through to stir to be mixed to obtain titanium alloy precision casting cladded type boron carbide base ceramic core material; Step 3, core material carried out to moulding, sintering obtains boron carbide base ceramic core; Sintering temperature is 1500 ~ 1900 DEG C, and the time is 0.5 ~ 20h.
3. the preparation method of titanium alloy precision casting cladded type boron carbide base ceramic core according to claim 2, it is characterized in that: the powder of the preparation rare earth oxide clad boron carbide described in step one, specifically comprise the steps: the first step, prepare boron carbide suspension: non-ionic surface active agent is joined in deionized water and form the first mixed solution, wherein contain 1-10g non-ionic surface active agent in every 100ml deionized water; Boron carbide powder is joined in the first mixed solution, stir and prepare boron carbide suspension; The addition of boron carbide powder adds 1 ~ 2mol in every 100ml deionized water; Second step, prepare rare earth oxide precursor solution: 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; 3rd step, rare earth oxide precursor solution is joined in boron carbide suspension, stir and obtain the second mixed solution; In the second described mixed solution, rare earth oxide presoma is 1:10-45 with the ratio of the mole of boron carbide powder; 4th step, ammoniacal liquor is added pH value to 8 ~ 11 adjusting solution in the second mixed solution obtain the 3rd mixed solution; 5th step, oven dry the 3rd mixed solution obtain drying powder; 6th step, by oven dry powder carry out sintering the powder obtaining rare earth oxide clad boron carbide; Described sintering, temperature is 1200-1600 DEG C, and the time is 0.5 ~ 20h.
4. the preparation method of titanium alloy precision casting cladded type boron carbide base ceramic core according to claim 3, is characterized in that: described inorganic zirconium salts is zirconium chloride or zirconium nitrate.
5. the preparation method of titanium alloy precision casting cladded type boron carbide base ceramic core according to claim 3, is characterized in that: described inorganic yttrium salts is yttrium chloride or yttrium nitrate.
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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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