CN1414145A - Growing technology of optical grade low corrusion tunnel density quartz crystal - Google Patents
Growing technology of optical grade low corrusion tunnel density quartz crystal Download PDFInfo
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- CN1414145A CN1414145A CN 02136142 CN02136142A CN1414145A CN 1414145 A CN1414145 A CN 1414145A CN 02136142 CN02136142 CN 02136142 CN 02136142 A CN02136142 A CN 02136142A CN 1414145 A CN1414145 A CN 1414145A
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- 239000013078 crystal Substances 0.000 title claims abstract description 89
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000010453 quartz Substances 0.000 title claims abstract description 40
- 230000003287 optical effect Effects 0.000 title claims abstract description 26
- 238000005516 engineering process Methods 0.000 title description 3
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000011044 quartzite Substances 0.000 claims description 10
- 239000001963 growth medium Substances 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 230000001186 cumulative effect Effects 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 238000007796 conventional method Methods 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 235000010288 sodium nitrite Nutrition 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- 241000220317 Rosa Species 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 description 17
- 239000008367 deionised water Substances 0.000 description 7
- 210000004907 gland Anatomy 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000013461 design Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000008239 natural water Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000003637 basic solution Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910001651 emery Inorganic materials 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000009605 growth rhythm Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- QFAXIZQBSCGJMA-UHFFFAOYSA-N mercury;hydrate Chemical compound O.[Hg] QFAXIZQBSCGJMA-UHFFFAOYSA-N 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
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Abstract
An optical-grade quartz crystal with low corrosion tunnel density is grown by hydrothermal differential-temp cyrstallizing method. It can be used for preparing low-corrosion filter for different cameras with high optical performance.
Description
The invention belongs to a kind of growth technique of quartz crystal, particularly a kind of growth technique that is applied to the optical grade low corrusion tunnel density quartz crystal of high precision optical filter elements such as digital camera, monitor, television telephone.
The synthetic quartz growth technique is to adopt hydrothermal temperature difference method to carry out in the autoclave of vertical sealing, because hydrothermal temperature difference method growth crystal is that growth is again to carry out under the physical and chemical condition of more complicated in basic solution, and its growth is again to finish in the autoclave of sealing, can not observe directly the whole process of growth, therefore, the grade of the quartz crystal that different growth techniques such as temperature and pressure control grow in the proportioning of different basic solutions and the autoclave is just different fully.Therefore the quartz crystal of producing in China's prior art is most of is the inferior grade quartz crystal, common the electronic component wafer as the piezoelectricity industry, civilian glasses lens, decoration jewellery or the like.These quartz crystals are of low grade, and output crosses Sheng, and cheap, manufacturing enterprise is almost profitless.And optical grade low corrusion tunnel density quartz crystal is a kind of quartz crystal materials that is applied to high precision optical filter elements such as digital camera, monitor, television telephone, and its price is 3 times of common crystalline, product 100% outlet, and supply falls short of demand in market.And present domestic synthetic quartzcrystal or only reach low corrusion tunnel density, but can not reach the optical grade standard; Maybe can reach the optical grade standard, but not reach low corrusion tunnel crystal standard, so China's optical grade low corrusion tunnel density quartz crystal element, main at present by import.
Task of the present invention provides a kind of employing hydro-thermal temperature difference crystallization process and grows a kind of quartz crystal, its index is reached: (1) corrusion tunnel density:＜100/cm
2, (2) Q value: 〉=2.6 * 10
6, (3) inclusion: more than the Ia class, (4) optical homogeneity: Δ n≤5 * 10
-6, (5) spectral transmittance (wavelength 800-2500mm):＞90%; It is a kind of optical grade low corrusion tunnel density quartz crystal that high precision optical filter elements such as digital camera, monitor, television telephone are used that is mainly used in.
Technical scheme of the present invention: the growth technique of optical grade low corrusion tunnel density quartz of the present invention is the hydro-thermal temperature difference crystallization process that adopts common quartz crystal: at first with seed crystal, quartzite raw material, ionized water (its specific conductivity＜3 * 10
6/ ohmcm) and growth media master liquid (Na2CO3, NaOH) equivalent concentration and additive Li (OH) 3, NaNO2 equivalent concentration screening, clean, preparation is ready to standby; Secondly former charging basket, seed crystal frame, plate washer, autoclave are cleaned by the traditional method of former common quartz crystal growth; In cleaned still, inject ready growth media then equally according to a conventional method, slowly put into charging basket that the quartzite raw material is housed and install the seed crystal frame that hangs with seed crystal, the still mouth is sealed on still top; After the dress still finishes, start temperature controlling system, the heating high-pressure still; The hydro-thermal temperature difference crystallization process of quartz crystal is to carry out under certain temperature and the pressure in autoclave, it is characterized in that:
A: seed crystal has at first screened optical grade low corrusion tunnel density less than 50/cm
2Quartz crystal adopts the high precision multi-cutting machine then, is 600 orders at subsidiary material silicon carbide, and rotating speed is to cut under 100 times/minute so slow low rate conditions, and the orientation accuracy that makes its seed crystal face was less than 5 minutes;
B: quartzite picking of raw material transparency is not less than 90%, silica composition is not less than 99.8%, and the granularity path length is the quartzite about 2cm;
C: it is 1.3N ± 0.1N that growth media (chemical reagent) adopts NaOH equivalent concentration, and additive adopts LiOHH
2O equivalent concentration is 0.07 ± 0.01N and NaNo
2Equivalent concentration is 0.05 ± 0.01N;
D: the compactedness in the still is 83%: liquor capacity should be effective volume and multiply by compactedness 83%, just V in the autoclave of promptly packing into
Water=(V
Cumulative volume in the still-V
The raw material basket is long-pending-V
The seed crystal support body is long-pending-V
The raw material volume-V
The seed crystal volume) 83%;
E: autoclave heating: at first adopting and making it after slowly heating up is that 345 ℃, bottom dissolve area (bottom placement quartzite raw material is as the nutrilite district autoclave in) temperature are that 380 ℃, autoclave base temperature are constant temperature 120 days under the condition of high voltage of 390 ℃ and pressure P=140mpa in vitellarium, top (autoclave upper suspension seed crystal district) temperature, and crystal growth temperature temperature difference control accuracy is ± 0.1 ℃;
F: slowly cooling is adopted in cooling, promptly with after reaching 120 hours with the high pressure temperature in the kettle and slowly reducing to 60 ℃, drives still and gets crystalline substance.
The every technical indicator of quartz crystal product of the growth technique growth of optical grade low corrusion tunnel density quartz crystal of the present invention all meets or exceeds GB GB7895-87 standard, and the requirement of user's particular technology index in the world, reach not defective of seed crystal, the gem-quality crystal of the optical grade low corrusion tunnel density that the outward appearance growth rhythm is neat.Its index: (1) corrusion tunnel density:＜100/cm
2, (2) Q value: 〉=2.6 * 10
6, (3) inclusion: more than the Ia class, (4) optical homogeneity Δ n≤5 * 10
-6(5) spectral transmittance (wavelength 800-2500mm):＞90%; Product lot quantity very exports.The low rotten filter element that utilizes the low rotten quartz crystal materials of this optical grade to make according to user's reflection is used in Electrofax, PC CCD camera, and system of supervision CCD camera, every technical indicator is stable on the video display telephone set, and effect is better.And low price but high quality is popular in users!
Below in conjunction with drawings and Examples the present invention is described in further detail
Fig. 1 is this quartz crystal technological process of production figure.
Fig. 2 is this quartz crystal growth temperature-rise period figure.
The key step of the growth technique of optical grade low corrusion tunnel density quartz crystal of the present invention is as follows as shown in the figure:
(1) preparatory stage:
1, seed crystal is exactly the crystal seed of synthetic quartzcrystal, at first will be according to the size processing seed crystal of crystal growth.
(1) seed screening low corrusion tunnel density itself is less than 50/cm
2Quartz crystal.
(2) adopted the high precision multi-cutting machine on the working method, subsidiary material silicon carbide is 600 orders, and rotating speed is 100 times/minute, cuts under so slow low rate condition, avoid seed crystal face to produce mechanical stress, for the crystal of growth optical grade low corrusion tunnel density is laid good basis.
(3) seed orientation: the orientation accuracy of seed crystal face was less than 5 minutes.
(4) seed crystal cleans: will cut directed good seed crystal and put into basin and deoil with the detergent immersion cleaning, clear water washes down then, the seed crystal that washes down is put into plastic tub, this is leaked basin place dense HF solution corrosion 1.5-2 hour, make seed crystal expose fresh, from HF solution, take out the leakage basin and place clear water to clean, after neutrality, take out the seed crystal dry for standby.
2, feedstock production: cultivate the natural quartz fragment of quartz crystal, often claim smelting quartz, adopt transparency to be not less than 90% usually, SiO
2Composition is not less than 99.8%, granularity is unsuitable excessive or too small, about path length 2cm for well, the picking raw material is chosen surface and the inner material piece that contains the impurity inclusion, the washing raw material, float surface impurity, smelting quartz after will cleaning again is placed in the Ultrasonic Cleaners and cleans, adds small amount of alkali, can take out raw material in 15 minutes from Ultrasonic Cleaners, crosses 2 times with deionized water after cleaning with flowing water again, and the raw material of the deionized water crossed is inserted dry for standby in the drying baker.
3, deionized water preparation: owing to contain the compound of salt such as Si, Fe, Al in the natural water, so use natural water.The tap water obtain solution, growth crystal will inevitably be brought a lot of foreign ions into, thereby influences quartzy quality, so must carry out purification process to natural water, makes deionized water, makes its electric conductivity＜3 * 10
-6/ ohmcm just can use.
4, growth media and additive are selected for use and prepared: it is that 1.3 ± 0.1N adopts additive also unusual that this technology growth media (chemical reagent) adopts NaOH equivalent concentration, this process using LiOHH
2O, NaNO
2Etc. multiple additives, LiOHH is used in apolegamy according to qualifications
2O equivalent concentration is 0.07 ± 0.01N, NaNO
2Equivalent concentration is 0.05 ± 0.01N.By different agent combination, select different equivalent concentration.
5, the cleaning of former charging basket, seed crystal frame, plate washer:
(1) former charging basket is clean with clear water and washed with de-ionized water with emery cloth polishing back earlier.
(2) mask pattern is all clean with pure water and washed with de-ionized water with emery cloth polishing back at every turn.
(3) baffle plate and seed crystal frame are one, and perforate is arranged on baffle plate.
6, autoclave cleans: clean still inwall secondary or wash away the still inwall with high pressure water mercury with clear water, nylon brush, remove the still wall dirt settling of remaining embryo and difference, use deionized water rinsing afterwards two times, it is stand-by to drain the interior residual water of still.
7, seed crystal hangs: hang seed crystal by design growing crystal scheme, every is left enough spaces all around to reach the size that the design crystal grows up to, and seed crystal is upper and lower to be twined with thin wire.
8, tightness system: check that whether whether sealing-ring reliably can have cut with reaching trim, coats molybdenumdisulphide to each parts thread part of autoclave then.
(2) the dress still stage:
The raw material of 1, will clean, drying (smelting quartz) is poured in the former charging basket by the raw material that design requirements takes by weighing certainweight, and charging basket is hung in the autoclave.
2, the solution for preparing is poured in the still.
3, clean seed crystal on seed crystal frame and the frame with pure water, put into still then.
4, measure the height of liquid level to the still mouth.Compactedness in the still is 83%, and liquor capacity should be effective volume and multiply by compactedness in the autoclave of promptly packing into, just V
Water=(V
Cumulative volume in the still-V
The raw material basket is long-pending-V
The seed crystal support body is long-pending-V
The raw material volume-V
The seed crystal volume) 83%;
5, sealing plug is hung in the still mouth, check its planeness.
6, big gland is screwed in kettle, after hand push is extremely tight, clash into big spanner with sledgehammer or weight again.The end tension of putting forth one's strength in addition of big spanner in order to avoid resilience, is clashed into big spanner and is rotated the gland angle and be about 60-90 ° and get final product.Reach and make wear ring outer ring and kettle sealing.
7, screw-in is carried the plug ring flange on sealing plug, mentions sealing plug to interior sealing station.
8, rotation is carried on the plug ring flange 8 and is carried the plug screw, mentions sealing plug and improves 2-3mm approximately and can reach and make between wear ring and sealing plug the effect of sealing mutually, and promptly wear ring reaches interior sealing.
9, the pressure measuring system device is installed.
10, still upper end heat-preservation cylinder is installed.Between tube inwall and kettle one lobe nut, hide, in case warm air convection current outside the space thus with woven asbesto.
(3) temperature rise period:
Fig. 2 crystal growth temperature-rise period (detailed description)
1, to begin be 60 ℃ to still internal upper part vitellarium temperature, rose to 250 ℃ in 20 hours, and this moment, constant temperature was 5 hours, rises to reach 330 ℃ in 20 hours again, and last slowly the intensification reached 345 ℃ of thermostat temperatures in 10 hours.
2, in the still bottom dissolve area temperature to begin be 60 ℃, in 20 hours, rise to 270 ℃, this moment, constant temperature was 5 hours, rose to reach 360 ℃ in 20 hours again, last slowly the intensification reached 380 ℃ of thermostat temperatures in 10 hours.
3, to begin be 60 ℃ to still inner bottom part dissolve area temperature, rose to 280 ℃ in 20 hours, and this moment, constant temperature was 5 hours, rises to reach 370 ℃ in 20 hours again, and last slowly the intensification reached 390 ℃ of thermostat temperatures in 10 hours.
(4) cultivation, crystallization, constant temperature stage:
After the dress still finishes, start temperature controlling system, the high pressure temperature in the kettle rises to: vitellarium, top temperature be 345 ℃, bottom dissolve area temperature be 380 ℃, bottom temp be 390 ℃ at constant temperature under the condition of high voltage of pressure 140Mpa about 120 days, cultivate quartz crystal, when crystal is in temperature constant state, crystal growth temperature and temperature difference control accuracy are ± 0.1 ℃, and the method growth of adopting the alternating temperature difference is to guarantee that optical homogeneity reaches higher service requirements (GB II level).
(5) temperature-fall period:
Behind the crystal growth end cycle, adopt slowly cooling, reduce to 60 ℃ of temperature in the kettle in 120 hours reaching, eliminate internal stress, to reach the optical grade low corrusion tunnel density standard quartz crystal.
(6) unload still and get crystalline substance:
1, waits that the crystal growth week after date that arrives design has a power failure cooling naturally.
When 2, the temperature on the kettle is reduced to 90 ℃, at each screw thread mouth place apply oil of kettle upper end, so that open autoclave.
The most suitable still of opening when 3, the temperature on the kettle is reduced to 60 ℃ takes off pressure tester (radiating pipe and tensimeter integral body are taken off from sealing plug).
When 4, driving still, unclamp 8 earlier and carry the plug screw, take out and carry the plug dish.
5, sealing plug is squeezed in the kettle, sealing plug and wear ring are broken away from, allow ring shrink and eliminate radial pressure.
6, put big spanner on the big gland, hit out big gland, screw out the 2-3 button then with sledgehammer or weight.
7, screw on and carry the plug dish and put on sealing plug, carry the plug screw with 8 again and screw in order to propose wear ring, ring and kettle potted line are broken away from, the ring outer gland sealing disappears.
8, the big gland extraction of closure plug of rotation, big tamponade, sealing cover, carry a cover system device such as plug dish.
9, take out crystal and place 50-60 ℃, clean crystal in the warm water.
10, quality inspection, classification, the branch specification check warehouse-in respectively of the crystal after will cleaning.
Claims (2)
1. the growth technique of an optical grade low corrusion tunnel density quartz is the hydro-thermal temperature difference crystallization process that adopts common quartz crystal: at first with seed crystal, quartzite raw material, ionized water (its specific conductivity＜3 * 10
6/ ohmcm) and growth media master liquid (Na2CO3, NaOH) equivalent concentration and additive Li (OH) 3, NaNO2 equivalent concentration screening, clean, preparation is ready to standby; Secondly former charging basket, seed crystal frame, plate washer, autoclave are cleaned by the traditional method of former common quartz crystal growth; In cleaned still, inject ready growth media then equally according to a conventional method, slowly put into charging basket that the quartzite raw material is housed and install the seed crystal frame that hangs with seed crystal, the still mouth is sealed on still top; After the dress still finishes, start temperature controlling system, the heating high-pressure still; The hydro-thermal temperature difference crystallization process of quartz crystal is to carry out under certain temperature and the pressure in autoclave, it is characterized in that:
A: seed crystal has at first screened optical grade low corrusion tunnel density less than 50/cm
2Quartz crystal adopts the high precision multi-cutting machine then, is 600 orders at subsidiary material silicon carbide, and rotating speed is to cut under 100 times/minute so slow low rate conditions, and the orientation accuracy that makes its seed crystal face was less than 5 minutes;
B: quartzite picking of raw material transparency is not less than 90%, silica composition is not less than 99.8%, and the granularity path length is the quartzite about 2cm;
C: it is 1.3N ± 0.1N that growth media (chemical reagent) adopts NaOH equivalent concentration, and additive adopts LiOHH
2O equivalent concentration is 0.07 ± 0.01N and NaNO
2Equivalent concentration is 0.05 ± 0.01N;
D: the compactedness in the still is 83%: liquor capacity should be effective volume and multiply by compactedness 83%, just V in the autoclave of promptly packing into
Water=(V
Cumulative volume in the still-V
The raw material basket is long-pending-V
The seed crystal support body is long-pending-V
The raw material volume-V
The seed crystal volume) 83%;
E: autoclave heating: at first adopting and making it after slowly heating up is that 345 ℃, bottom dissolve area (bottom placement quartzite raw material is as the nutrilite district autoclave in) temperature are that 380 ℃, autoclave base temperature are constant temperature 120 days under the condition of high voltage of 390 ℃ and pressure P=140mpa in vitellarium, top (autoclave upper suspension seed crystal district) temperature, and crystal growth temperature temperature difference control accuracy is ± 0.1 ℃;
F: slowly cooling is adopted in cooling, promptly with after reaching 120 hours with the high pressure temperature in the kettle and slowly reducing to 60 ℃, drives still and gets crystalline substance.
2, according to the growth technique of the described a kind of optical grade low corrusion tunnel density quartz of claim 1, it is characterized in that: it is 60 ℃ that crystal growth temperature-rise period (1) still internal upper part vitellarium temperature begins, in 20 hours, rise to 250 ℃, this moment, constant temperature was 5 hours, rise and reached 330 ℃ in 20 hours, last slowly the intensification reached 345 ℃ of thermostat temperatures in 10 hours; (2) in the still bottom dissolve area temperature to begin be 60 ℃, in 20 hours, rise to 270 ℃, this moment, constant temperature was 5 hours, rose to reach 360 ℃ in 20 hours again, last slowly the intensification reached 380 ℃ of thermostat temperatures in 10 hours; (3) to begin be 60 ℃ to still inner bottom part dissolve area temperature, rose to 280 ℃ in 20 hours, permanent 5 hours of this moment rose and reached 370 ℃ in 20 hours, and last slowly the intensification reached 390 ℃ of thermostat temperatures in 10 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02136142 CN1207447C (en) | 2002-07-17 | 2002-07-17 | Growing technology of optical grade low corrusion tunnel density quartz crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02136142 CN1207447C (en) | 2002-07-17 | 2002-07-17 | Growing technology of optical grade low corrusion tunnel density quartz crystal |
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| Publication Number | Publication Date |
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| CN1414145A true CN1414145A (en) | 2003-04-30 |
| CN1207447C CN1207447C (en) | 2005-06-22 |
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|---|---|---|---|
| CN 02136142 Expired - Fee Related CN1207447C (en) | 2002-07-17 | 2002-07-17 | Growing technology of optical grade low corrusion tunnel density quartz crystal |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100335683C (en) * | 2005-05-20 | 2007-09-05 | 淄博宇峰实业有限责任公司 | Method for preparing large-size artificial optical quartz crystal by hydrothermal method |
| CN100400718C (en) * | 2005-05-20 | 2008-07-09 | 淄博宇峰实业有限责任公司 | Growth method for single-side optical crystal |
| CN101319374B (en) * | 2008-05-08 | 2010-07-28 | 刘盛浦 | Optical-level single-sided long quartz crystal growth technique |
| CN101319375B (en) * | 2008-05-08 | 2010-09-22 | 刘盛浦 | Optical-level quartz crystal temperature-variable temperature difference method growth technique |
| CN101323976B (en) * | 2008-07-30 | 2011-04-13 | 常州松晶电子有限公司 | Production method of non-inoculating crystal sonic surface wave quartz crystal |
| CN101052753B (en) * | 2004-09-13 | 2012-01-04 | 岛根县 | Method for manufacturing porous silica crystal |
| CN101311368B (en) * | 2008-04-29 | 2012-08-15 | 烁光特晶科技有限公司 | Growth method of quartz crystal |
| CN104109900A (en) * | 2014-06-17 | 2014-10-22 | 北京石晶光电科技股份有限公司济源分公司 | Growth method of novel piezoelectric crystal for surface acoustic waves, dedicated separation blade and dedicated crystal rack |
| CN109137074A (en) * | 2018-10-23 | 2019-01-04 | 梁维嘉 | The artificial culture growing method of quartzy embryo |
| CN112899778A (en) * | 2021-01-21 | 2021-06-04 | 烁光特晶科技有限公司 | Method for manufacturing deep ultraviolet high-transmittance quartz crystal |
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2002
- 2002-07-17 CN CN 02136142 patent/CN1207447C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101052753B (en) * | 2004-09-13 | 2012-01-04 | 岛根县 | Method for manufacturing porous silica crystal |
| CN100335683C (en) * | 2005-05-20 | 2007-09-05 | 淄博宇峰实业有限责任公司 | Method for preparing large-size artificial optical quartz crystal by hydrothermal method |
| CN100400718C (en) * | 2005-05-20 | 2008-07-09 | 淄博宇峰实业有限责任公司 | Growth method for single-side optical crystal |
| CN101311368B (en) * | 2008-04-29 | 2012-08-15 | 烁光特晶科技有限公司 | Growth method of quartz crystal |
| CN101319374B (en) * | 2008-05-08 | 2010-07-28 | 刘盛浦 | Optical-level single-sided long quartz crystal growth technique |
| CN101319375B (en) * | 2008-05-08 | 2010-09-22 | 刘盛浦 | Optical-level quartz crystal temperature-variable temperature difference method growth technique |
| CN101323976B (en) * | 2008-07-30 | 2011-04-13 | 常州松晶电子有限公司 | Production method of non-inoculating crystal sonic surface wave quartz crystal |
| CN104109900A (en) * | 2014-06-17 | 2014-10-22 | 北京石晶光电科技股份有限公司济源分公司 | Growth method of novel piezoelectric crystal for surface acoustic waves, dedicated separation blade and dedicated crystal rack |
| CN109137074A (en) * | 2018-10-23 | 2019-01-04 | 梁维嘉 | The artificial culture growing method of quartzy embryo |
| CN112899778A (en) * | 2021-01-21 | 2021-06-04 | 烁光特晶科技有限公司 | Method for manufacturing deep ultraviolet high-transmittance quartz crystal |
| CN112899778B (en) * | 2021-01-21 | 2022-02-01 | 烁光特晶科技有限公司 | Method for manufacturing deep ultraviolet high-transmittance quartz crystal |
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