CN103046137A - Sapphire crystal with high mechanical property and fabrication method thereof - Google Patents
Sapphire crystal with high mechanical property and fabrication method thereof Download PDFInfo
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Abstract
The invention relates to a sapphire crystal with a high mechanical property and a fabrication method thereof. The sapphire crystal with the high mechanical property is doped with carbon and titanium; the doping content of the carbon is 1,000-10,000ppm of the total mass of the crystal; and the doping content of the titanium is 500-3,000ppm of the total mass of the crystal. The invention further discloses the fabrication method of the crystal, which comprises the following steps: mixing raw materials at a mixture ratio, grinding, conducting a forming technology, fabricating a crystal growth raw material, and growing the crystal by a temperature gradient method, a descent method or a kyropoulos method. The sapphire crystal doped with the carbon and the titanium is higher in surface hardness, breaking strength and breaking tenacity; and doping ions do not damage optical permeability of the sapphire crystal.
Description
Technical field
The present invention relates to a kind of sapphire crystal, relate in particular to a kind of sapphire crystal with good mechanical property and preparation method thereof.
Background technology
Sapphire crystal, because of its wide band high transmission performance and relative superior comprehensive physical and chemical performance, makes it in modern national defense science and civilian technology Application Areas, important value be arranged.In the military electro-optical equipment field: the infrared optical window made from sapphire crystal and nose cone, airborne, spaceborne, carrier-borne and latent base, continental rise optoelectronic device have been widely used in, especially the status in the military equipments such as High Mach number guided missile dome, transparent armor, submarine window and high power strong laser and act on irreplaceable.At civil area: sapphire crystal is because having wide band perviousness, high strength, high temperature resistant, wear-resistant, corrosion-resistant, and can be used as the equipment of working or view port and the detection window of instrument under the severe environment such as various high temperature, high pressure, as: resistant to elevated temperatures thermopair and boiler water gauge, anti abrasive bar code scanner window, the sensor that coal, gas, oil well detection high temperature resistant and corrosion are used and detector window etc.; But sapphire crystal equally also exists native defect, because sapphire crystal is typical covalent linkage, there is obvious directivity, the jack per line ion meets, and repulsion is very big; And sapphire crystal belongs to corundum type structure, trigonal system R-3C symmetry, the crystalline structure complexity, its crystals does not have sliding system, there is the shortcoming of brittle rupture under the aerothermal impact in the external world, this is a sapphire crystal material large weakness in actual applications, has limited the application and development of sapphire crystal in wider field.And, under the hot environment action of compressive stress, sapphire crystal r face easily produces twin, under stress, twin is loosening, causes its flexural strength the shortcoming descended rapidly to occur.
In sum, the weakness of sapphire crystal mechanical property has restricted this crystal further at the application and development in wider field, and therefore, developing high-strength mechanical property sapphire crystal has become the problem that those skilled in the art need solution badly.
Based on sapphire crystal mechanical property defect people, multiple solution has been proposed, as in U.S. Pat 5702654, technology point is: the MgO powder is covered on sapphire, and be heated to certain temperature (1500 ℃ ~ 1750 ℃) and keep certain hour under the environment of atmosphere or logical argon gas, make Mg
2+produce surface diffusion, then the MgO powder is removed, use instead after the second temperature (1800 ℃ ~ 2000 ℃) is incubated certain hour and make surperficial Mg
2+be evenly distributed in the full wafer crystal, through after a while by Mg
2+crystal after homogenizing is annealed to the third temperature (1200 ℃ ~ 1450 ℃) rapidly, then is annealed or timeliness with this temperature, so that the second-phase of precipitation-hardening is strengthened sapphire.Although the method can improve the mechanical property of sapphire crystal to a certain extent, only to reach the purpose of strengthening be inadequate to the way by surface modification, and Mg
2+approximately in 2000 ℃ of high temperature annealings, being easy to volatilization, do not reach the purpose of expection.And, in U.S. Pat 6222194B1, the method for employing is: adopt fast neutron irradiated strengthening sapphire, the energy of fast neutron is greater than 0.1MeV, and the irradiation injection rate is 1 * 10
14~ 9 * 10
19neutron/cm
2.In irradiation process, sapphire crystal is by 10B and Cd parcel, to remove the impact of thermal neutron.When through 1 * 10
18neutrons/cm
2fast neutron irradiated after, because fast neutron irradiated has hindered the formation of twin, therefore the c-axis intensity of crystal has improved 3 times at 600 ℃.The method can't meet the large-size sapphire radiation parameter due to high cost and equipment, also can't carry out the industry application of scale.Based on above-mentioned background, improving the technical significantly deficiency that still exists of sapphire crystal mechanical property, be difficult to reach the required requirement of industrial production at present.
Summary of the invention
The purpose of this invention is to provide a kind of high-strength mechanical property sapphire crystal and preparation method thereof.To be solved by this invention is the problem of current sapphire crystal mechanical property Shortcomings.
To achieve these goals, the technical solution used in the present invention is as follows:
First aspect of the present invention provides a kind of high-strength mechanical property sapphire crystal, the sapphire crystal that described crystal is the doping carbon titanium elements, wherein, 1000 ~ 10000ppm that the carbon doping is the crystal total mass, 500 ~ 3000ppm that titanium doped amount is the crystal total mass.
Described high-strength mechanical property sapphire crystal is preferably according to the described method preparation in second aspect of the present invention.
Second aspect of the present invention is to provide a kind of method for preparing high-strength mechanical property sapphire crystal, and described method comprises the steps:
Step 1,500 ~ 3000ppm that the 1000 ~ 10000ppm that is the crystal total mass according to the carbon doping, titanium doped amount are the crystal total mass provides α-Al
2o
3base starting material, titanium source and carbon source; Batch mixing, grinding and moulding process make the crystal growth raw material;
Wherein, the titanium source is preferably TiO
2.
Wherein, carbon source is preferably graphite carbon.
In second described method in aspect of the present invention, described in step 1, moulding process is preferably cold isostatic compaction.
In second described method in aspect of the present invention, in step 2, can adopt warm terraced method or descent method or kyropoulos growing technology to make crystal.
Preferably, the concrete steps of the terraced method growing crystal of described temperature are: put into seed crystal in the container seed slot, the crystal growth raw material is put into to container; ≤ 5 * 10
-3under Pa pressure, persistently overheating to 2333 ~ 2363K, after crystal growth raw material fusing, constant temperature 1 ~ 3h is to fusing fully, then with the speed cooling growing crystal of 1 ~ 5K/h; After growth finishes, the crystal of taking-up after the air atmosphere annealing 48 ~ 72h of 1873K ~ 2073K temperature, is down to room temperature again.
Described container is preferably crucible, and more preferably molybdenum crucible, tungsten and molybdenum crucible, tungsten crucible, most preferably be molybdenum crucible.
Described seed crystal is preferably the sapphire crystal of [11-20] direction.
Preferably, the concrete steps of described descent method for growing crystal are: put into seed crystal in the container seed slot, the crystal growth raw material is put into to container; ≤ 5 * 10
-3under Pa pressure, persistently overheating to 2333 ~ 2363K, after after the raw material fusing, constant temperature 3 ~ 5h melts fully, with the speed decline container growing crystal of 0.3 ~ 1mm/h; After growth finishes, the crystal of taking-up after the air atmosphere annealing 48 ~ 72h of 1873K ~ 2073K temperature, is down to room temperature again.
Described container is preferably crucible, and more preferably molybdenum crucible, tungsten and molybdenum crucible, tungsten crucible, most preferably be tungsten and molybdenum crucible.
Described seed crystal is preferably the sapphire crystal of [11-20] direction.
Preferably, in the process of above-mentioned descent method for growing crystal, the growth interface thermograde is preferably 30 ~ 40K/cm.
Preferably, the concrete steps of described kyropoulos growing crystal are: the crystal growth raw material is put into to container, and seed crystal hangs on the positive upper end of container, sealing; ≤ 5 * 10
-3under Pa pressure, persistently overheating to 2333 ~ 2383K, constant temperature 3 ~ 8h after raw material melts fully, be cooled near fusing point and by the seed crystal slow decreasing, make it to contact with melt liquid level in container, carry out the operation of necking down seeding after seed end and the complete welding of melt, then with the cooling rate of 0.05 ~ 3mm/h pull rate, 0.1 ~ 1.5K/h, carry out crystal shouldering and isodiametric growth.Crystallization is down to room temperature with 5～35K/h speed after finishing.The crystal taken out passes through the air atmosphere annealing 48 ~ 72h of 1873K ~ 2073K temperature again.
Described container is preferably crucible, and more preferably molybdenum crucible, tungsten and molybdenum crucible, tungsten crucible, most preferably be tungsten crucible.
Described seed crystal is preferably the sapphire crystal of [11-20] direction.
The invention provides a kind of high-strength mechanical property sapphire crystal, this crystal in sapphire (sapphire) crystal, adulterate high-purity graphite carbon and the titanium dioxide of certain mass mark, adopt warm terraced method or descent method or kyropoulos technology growth to obtain sapphire (C, the Ti:sapphire) crystal of doping carbon titanium elements.Enter interstitial void by carbon ion and form the interstitial carbon ion, the cracking of gap ion pair sapphire single-crystal has pinning effect, improved the fracture surface energy of crystal, reach the effect of highly malleablized sapphire single-crystal under normal temperature, simultaneously, the titanic ion solid solution of doping enters matrix trivalent aluminium ion case, form non-equivalence and not isometrical metalepsy, cause lattice imperfection and lattice distortion and form new stress field, improved Young's modulus and the fracture surface energy of sapphire crystal, sapphire crystal has been played to strengthening mechanism.With the normal blue gem crystal, compare, C of the present invention, the Ti:sapphire crystal has significantly more surface hardness, breaking tenacity and the fracture toughness property of Gao Gengqiang, and the carbon titanium ion of doping does not damage the through performance of sapphire crystal, for sapphire crystal provides wider space as window material or substrate material.
The accompanying drawing explanation
The C made in Fig. 1 embodiment 1, the surface hardness of Ti:sapphire crystal;
The C made in Fig. 2 embodiment 1, the breaking tenacity of Ti:sapphire crystal;
The C made in Fig. 3 embodiment 1, the fracture toughness property of Ti:sapphire crystal;
The C made in Fig. 4 embodiment 1, the absorption spectrum curve of Ti:sapphire crystal.
Embodiment
The invention provides a kind of sapphire crystal of doping carbon titanium of high-strength mechanical property, with Al
2o
3for substrate material, the carbon doping is 1000 ~ 10000ppm, and titanium doped amount is 500 ~ 3000ppm.Under normal temperature, its surface hardness reaches 1900 ~ 2200Kg/mm
2, breaking tenacity reaches 600 ~ 800MPa, and fracture toughness property reaches 2.6 ~ 3.0MPa
.m
1/2.
Further set forth the present invention below in conjunction with embodiment.Should be understood that these embodiment are only for the present invention is described, but not limit the scope of the invention.
embodiment 1: warm terraced method grow doping amount is 5000ppm graphite carbon and 1000ppmTiO
2
c, the Ti:sapphire crystal
Take respectively α-Al that purity is 99.999%
2o
3raw material 3Kg, the spectroscopically pure TiO of 1000ppm
2(being 3g), and 5000ppm spectroscopically pure graphite carbon (being 15g), mixed grinding 24h on planetary ball mill, after taking out cold dry-pressing formed be that the piece material is standby.
Adopt warm terraced method growth C, the Ti:sapphire crystal, concrete steps are: select a to do seed crystal to [11-20] ethereal blue jewel, put into ethereal blue jewel seed crystal in the molybdenum crucible seed slot, the piece material suppressed is put into to crucible uniformly, cover crucible cover, shove charge.Be evacuated to furnace pressure<5 * 10
-3pa, persistently overheating to 2333K, constant temperature 3h after raw material fusing, after melt melts fully and stablize, start slow crystallization with the speed of the 1K/h melt of lowering the temperature by the seed crystal place, until the complete crystallization of melt, speed with 40K/h is cooled to room temperature taking-up crystal, and the crystal of taking-up is process 1973K air atmosphere annealing 60h again, then is cooled to room temperature with the speed of 35K/h, make C, the Ti:sapphire crystal.
The C that growth obtains, the Ti:sapphire crystal perfection, without the obviously appearance of wrap and bubble, crystal shows slightly blush, cut into respectively sheet and strip crystal along basal plane [0001], normal temperature surface hardness, breaking tenacity and the fracture toughness property of sample after polishing are measured.
Fig. 1 is the C made in the present embodiment, the normal temperature c face surface hardness test result of Ti:sapphire crystal.With pure sapphire average surface hardness 1701 Kg/mm
2compare, C, the average surface hardness of Ti:sapphire crystal obviously improves, and reaches 2031Kg/mm
2.Fig. 2 and Fig. 3 are C, Ti:sapphire crystal breaking tenacity and fracture toughness property test result at normal temperatures, and the sample measurement dimensional standard is 4mm * 36mm (C face) * 3mm, result shows the 1000ppmTiO that adulterates
2with its breaking tenacity of sapphire of 5000ppm graphite carbon, improve a lot, and fracture toughness property is also significantly optimized.The normal temperature breaking tenacity observed value average out to 492Mpa of pure sapphire crystal, doping C, Ti:sapphire crystalline fracture intensity level on average reaches 703MPa, and fracture toughness property is by the average 1.81Mpa of pure sapphire
.m
1/2be optimized to average 2.77 MPa
.m
1/2.Simultaneously dopant ion can not damage the optical transmittance of sapphire crystal, and Fig. 4 is the C made in the present embodiment, the visible-near-infrared spectrum of Ti:sapphire crystal see through spectrogram, its transmitance at visible-near-infrared spectrum reaches 80%.C prepared by the present embodiment, the Ti:sapphire crystal has high-strength Mechanical Characteristics, has guaranteed the good spectrum through performance of crystal simultaneously, in window material field and substrate material field, is with a wide range of applications.
embodiment 2: warm terraced method grow doping amount is 1000ppm graphite carbon and 500ppmTiO
2
c, the Ti:sapphire crystal
Except the doped graphite carbon that adds is that 1000ppm(is 3g), and doped Ti O
2for 500ppm(is 1.5g) in addition, other are prepared burden with embodiment 1, mixed grinding 24h on planetary ball mill, after taking out cold dry-pressing formed be that the piece material is standby.
Adopt warm terraced method growth C, the Ti:sapphire crystal, concrete steps are: select a to do seed crystal to [11-20] ethereal blue jewel, put into the sapphire seed crystal in the seed slot of molybdenum crucible, the piece material suppressed is put into to crucible uniformly, cover crucible cover, shove charge.Be evacuated to furnace pressure<5 * 10
-3pa, persistently overheating to 2363K, constant temperature 1h after raw material fusing, after melt melts fully and stablize, start slow crystallization with the speed of the 1.5K/h melt of lowering the temperature by the seed crystal place, until the complete crystallization of melt, speed with 35K/h is cooled to room temperature taking-up crystal, and the crystal of taking-up is process 1873K air atmosphere annealing 48h again, then is cooled to room temperature with the speed of 40K/h, make C, the Ti:sapphire crystal.
embodiment 3: warm terraced method grow doping amount is 10000ppm graphite carbon and 3000ppmTiO
2
c, the Ti:sapphire crystal
Except the doped graphite carbon that adds is that 10000ppm(is 30g), and doped Ti O
2for 3000ppm(is 9g) in addition, other are prepared burden with embodiment 1, mixed grinding 24h on planetary ball mill, after taking out cold dry-pressing formed be that the piece material is standby.
Adopt warm terraced method growth C, the Ti:sapphire crystal, concrete steps are: select a to do seed crystal to [11-20] ethereal blue jewel, put into the Sapphire seed crystal in the seed slot of molybdenum crucible, the piece material suppressed is put into to crucible uniformly, cover crucible cover, shove charge.Be evacuated to furnace pressure<5 * 10
-3pa, persistently overheating to 2348K, constant temperature 2h after raw material fusing, after melt melts fully and stablize, start slow crystallization with the speed of the 2K/h melt of lowering the temperature by the seed crystal place, until the complete crystallization of melt, speed with 45K/h is cooled to room temperature taking-up crystal, and the crystal of taking-up is process 2073K air atmosphere annealing 72h again, then is cooled to room temperature with the speed of 38K/h, make C, the Ti:sapphire crystal.
embodiment 4: the descent method for growing doping is 5000ppm graphite carbon and 1000ppmTiO
2
c, the Ti:sapphire crystal
Taking respectively purity is 99.999% α-Al
2o
310Kg, 5000ppm spectroscopically pure graphite carbon (being 50g), and the spectroscopically pure TiO of 1000ppm
2(being 10g), mixed grinding 24h on planetary ball mill, after taking out cold dry-pressing formed be that the piece material is standby.
Adopt descent method for growing C, the Ti:sapphire crystal, concrete steps are: the crystal growth raw material mixed is put into to crucible, cover crucible cover, shove charge, be evacuated to furnace pressure<5 * 10
-3pa, persistently overheating to 2353K, constant temperature 4h after raw material fusing, after melt melts fully and stablizes, keeping the growth interface thermograde is 35K/cm, then the speed decline crucible with 0.6mm/h starts crystalline growth, until the complete crystallization of melt, is cooled to room temperature with the speed of 35K/h and takes out crystal, the crystal taken out is again through 1973K air atmosphere annealing 60h, speed with 35K/h is cooled to room temperature again, makes C, the Ti:sapphire crystal.
embodiment 5: kyropoulos grow doping amount is 5000ppm graphite carbon and 1000ppmTiO
2
c, the Ti:sapphire crystal
Taking respectively purity is 99.999% α-Al
2o
330Kg, 5000ppm spectroscopically pure graphite carbon (being 150g), and the spectroscopically pure TiO of 1000ppm
2(being 30g), mixed grinding 24h on planetary ball mill, after taking out cold dry-pressing formed be that the piece material is standby.
Adopt kyropoulos growth C, the Ti:sapphire crystal, concrete steps are: the crystal growth raw material is put into to tungsten crucible, crucible is packed in burner hearth, the Al of [11-20] direction
2o
3seed crystal is fixed in seed chuck and is placed in directly over crucible, builds bell sealing.Be evacuated to furnace pressure lower than 5 * 10
-3pa, persistently overheating to 2373K, constant temperature 5h after raw material melts fully, progressively be cooled near fusing point, then the seed crystal slow decreasing is made it to contact with melt liquid level, note observing the thawing of seed end, after seed end and the complete welding of melt, carry out the operation of necking down seeding, then with the cooling rate of 0.1 ~ 0.3mm/h pull rate, 0.6 ~ 1K/h, carry out crystal shouldering and isodiametric growth.After growth finishes, be down to room temperature with 20K/h speed and take out crystal, the crystal of taking-up is process 2000K air atmosphere annealing 72h again, then is cooled to room temperature with the speed of 30K/h, makes C, the Ti:sapphire crystal.
Above specific embodiments of the invention be have been described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and alternative also all among category of the present invention.Therefore, equalization conversion and the modification done without departing from the spirit and scope of the invention, all should contain within the scope of the invention.
Claims (12)
1. a high-strength mechanical property sapphire crystal,, it is characterized in that, the sapphire crystal that described crystal is the doping carbon titanium elements, wherein, 1000 ~ 10000ppm that the carbon doping is the crystal total mass, 500 ~ 3000ppm that titanium doped amount is the crystal total mass.
2. sapphire crystal according to claim 1, is characterized in that, described Al
2o
3for α-Al
2o
3.
3. a method for preparing high-strength mechanical property sapphire crystal, is characterized in that, described method comprises the steps:
Step 1,500 ~ 3000ppm that the 1000 ~ 10000ppm that is the crystal total mass according to the carbon doping, titanium doped amount are the crystal total mass provides α-Al
2o
3base starting material, titanium source and carbon source; Batch mixing, grinding and moulding process make crystal growth raw material piece material;
Step 2, growth obtains crystal.
4. method according to claim 3, is characterized in that, described titanium source is TiO
2.
5. method according to claim 3, is characterized in that, described carbon source is graphite carbon.
6. method according to claim 3, is characterized in that, described in step 1, moulding process is preferably cold isostatic compaction.
7. according to the described method of any one in claim 3 ~ 6, it is characterized in that, in step 2, adopt warm terraced method or descent method or kyropoulos growing technology to make crystal.
8. method according to claim 7, is characterized in that, the concrete steps of the terraced method growing crystal of described temperature are: put into seed crystal in the container seed slot, the crystal growth raw material is put into to container; ≤ 5 * 10
-3under Pa pressure, persistently overheating to 2333 ~ 2363K, after crystal growth raw material fusing, constant temperature 1 ~ 3h is to fusing fully, then with the speed cooling growing crystal of 1 ~ 5K/h; After growth finishes, the crystal of taking-up after the air atmosphere annealing 48 ~ 72h of 1873K ~ 2073K temperature, is down to room temperature again.
9. method according to claim 7, is characterized in that, the concrete steps of described descent method for growing crystal are: put into seed crystal in the container seed slot, the crystal growth raw material is put into to container; ≤ 5 * 10
-3under Pa pressure, persistently overheating to 2333 ~ 2363K, after after the raw material fusing, constant temperature 3 ~ 5h melts fully, with the speed decline container growing crystal of 0.3 ~ 1mm/h; After growth finishes, the crystal of taking-up after the air atmosphere annealing 48 ~ 72h of 1873K ~ 2073K temperature, is down to room temperature again.
10. method according to claim 9, is characterized in that, the growth interface thermograde is 30 ~ 40K/cm.
11. method according to claim 7, is characterized in that, the concrete steps of described kyropoulos growing crystal are: the crystal growth raw material is put into to container, and seed crystal hangs on the positive upper end of container, sealing; ≤ 5 * 10
-3under Pa pressure, persistently overheating to 2333 ~ 2383K, constant temperature 3 ~ 8h after raw material melts fully, be cooled near fusing point and by the seed crystal slow decreasing, make it to contact with melt liquid level in container, carry out the operation of necking down seeding after seed end and the complete welding of melt, then with the cooling rate of 0.05 ~ 3mm/h pull rate, 0.1 ~ 1.5K/h, carry out crystal shouldering and isodiametric growth;
Crystallization is down to room temperature with 5～35K/h speed after finishing;
The crystal taken out passes through the air atmosphere annealing 48 ~ 72h of 1873K ~ 2073K temperature again.
12. according to Claim 8 ~ 11, the described method of any one, is characterized in that, the sapphire crystal that described seed crystal is [11-20] direction.
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| CN107937983A (en) * | 2018-01-04 | 2018-04-20 | 河北工业大学 | A kind of sapphire material of multicomponent doping and its preparation method and application |
| CN110528076A (en) * | 2019-10-08 | 2019-12-03 | 四川大学 | A kind of sapphire and graphene doping generate sapphire method |
| CN112979288A (en) * | 2021-02-09 | 2021-06-18 | 洛阳润宝研磨材料有限公司 | Preparation method of sapphire grinding material |
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| CN105830137B (en) * | 2013-12-21 | 2019-06-14 | 京瓷株式会社 | The translucent cover component of electronic equipment and electronic equipment |
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| CN110528076A (en) * | 2019-10-08 | 2019-12-03 | 四川大学 | A kind of sapphire and graphene doping generate sapphire method |
| CN112979288A (en) * | 2021-02-09 | 2021-06-18 | 洛阳润宝研磨材料有限公司 | Preparation method of sapphire grinding material |
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| CN113252176A (en) * | 2021-04-30 | 2021-08-13 | 太原理工大学 | Sapphire inoculation point high-precision sensing device and method based on radiation spectrum |
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