CN101319375B - Optical-level quartz crystal temperature-variable temperature difference method growth technique - Google Patents
Optical-level quartz crystal temperature-variable temperature difference method growth technique Download PDFInfo
- Publication number
- CN101319375B CN101319375B CN2008100160202A CN200810016020A CN101319375B CN 101319375 B CN101319375 B CN 101319375B CN 2008100160202 A CN2008100160202 A CN 2008100160202A CN 200810016020 A CN200810016020 A CN 200810016020A CN 101319375 B CN101319375 B CN 101319375B
- Authority
- CN
- China
- Prior art keywords
- hours
- temperature
- rises
- days
- rose
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Abstract
The invention discloses an optical level quartz crystal temperature-changing temperature differential method growth technology, comprising the following steps that: firstly, raw materials of seed crystal and quartzite are washed, deionized water and a growth-promoting media are prepared, and a high-pressure autoclave is washed by ionized water and is drained off by a membrane pump; secondly, a raw material basket holding the quartzite is put in the washed autoclave, the prepared grow-promoting media and a seed crystal bracket hung with the seed crystal are poured into the autoclave, the liquid level is measured, and the autoclave opening is sealed; thirdly, a temperature control system is started, the high-pressure autoclave is heated, the parameters of temperature, pressure and time of the sealed high-pressure autoclave are adjusted so that the quartz crystal is grown and formed. The optical level quartz crystal temperature-changing temperature differential method growth technology is characterized by determining the lineage grade of the seed crystal, the a equivalent concentration of the grow-promoting media, the parameter of a filling degree of the autoclave, the temperature changing and differential parameter and the pressure parameter of the heated high-pressure autoclave. According to the quartz crystal produced by the technology, the lineage index is more than the gradeA, the etch channel density is less than 10 strips per centimeter<2>, the value of Q is more than or equal to 3.0x10<6>, an inclusion is higher than the Ia type, the optical uniformity delta n is less than or equal to 5x10<-6>, and the spectrum transmission ratio is more than 95 percent when the wavelength is between 800 and 2, 500 nanometers.
Description
Technical field
The present invention relates to the growth technique of quartz crystal, particularly relate to technology with the brilliant method of hydro-thermal thermal junction growing optics level quartz crystal in autoclave.
Background technology
Artificial quartz crystal growth's technology is to adopt hydrothermal temperature difference method to realize in the autoclave of vertical sealing.Because hydrothermal temperature difference method growth quartz 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, therefore can not observe directly the whole process of growth.And the proportioning of different basic solutions, the choosing of compactedness parameter in the still, the control of temperature, time, pressure parameter etc. all can produce material impact to the grade of the quartz crystal that grows again during the autoclave heating.This has just increased the difficulty of such subject study test to a great extent.Current, the quartz crystal that China grows in autoclave with the brilliant method of hydro-thermal thermal junction mostly is the quartz crystal of lower grade greatly, is applied to the piezoelectricity industry usually.And optical-level 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, even and some index of synthetic quartzcrystal of domestic enterprise's production at present meets the requirements, also be difficult to reach fully the optical grade standard.Though countries such as the U.S., Japan, Canada can produce the quartz crystal materials of optical grade, qualification rate is all also very low.By the applicant of present patent application in application on July 17th, 2002, Granted publication number discloses a kind of growth technique of optical grade low corrusion tunnel density quartz crystal for the patent of invention of CN1207447C, though also can reach the requirement of optical-level quartz crystal material with the quartz crystal of this explained hereafter, but along with the fast development of digital product in recent years, particularly along with ten million pixel photovoltaic, the appearance of ray machine electricity product, again new requirement has been proposed the optical-level quartz crystal material, except in crystal to the index request strictnesses such as inclusion, also arteries and veins reason index has been proposed quartz crystal.It is the also strict optical-level quartz crystal product of A level, other leading indicator that existing production technique is difficult to produce arteries and veins reason index, and domestic and international many enterprises also are attempts to address this problem with temperature-variable temperature difference method growth technique, but fails of the effect.
Summary of the invention
Purpose of the present invention will provide a kind of improved optical-level quartz crystal temperature-variable temperature difference method growth technique exactly, it can solve effectively adopts existing technology to be difficult to satisfy the problem that optical-level quartz crystal is managed index, inclusion index, corrusion tunnel density index, Q value index, optical homogeneity index, spectral transmittance index high performance requirements to arteries and veins, also can further solve existing optical-level quartz crystal simultaneously and be difficult to meet the problem of high-tech products such as digital camera, monitor, television telephone to high pixel request.
The object of the present invention is achieved like this: optical-level quartz crystal temperature-variable temperature difference method growth technique, at first clean seed crystal, quartzite raw material, preparation deionized water and growth media, drain with ionized water cleaning autoclave and with surge pump, in cleaned still, put into the former charging basket that quartzite is housed then, inject growth media that has prepared and the seed crystal frame that hangs with seed crystal, measured liquid level, the still mouth is sealed, restart temperature controlling system, the heating high-pressure still is adjusted temperature, pressure, time parameter to the autoclave of sealing, make the quartz crystal growth shaping, it is characterized in that
A, seed crystal select optical-level quartz crystal arteries and veins reason to be the A level;
B, growth media are that NaOH and the equivalent concentration of 1.2 ± 0.1mol/L is the LiOHH of 0.07 ± 0.01mol/L by equivalent concentration
2O, NaNO
2Form;
Compactedness satisfies V in c, the still
Liquid=(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 volumeThe % of) * (83-84);
D, autoclave heating:
Point for measuring temperature T is set from top to bottom in the vitellarium
1And T
2, point for measuring temperature T is set from top to bottom at dissolve area
3, T
4And T
5, the temperature and time parameter control in autoclave when heating, wherein temperature range be controlled at ± 3 ℃, the time parameter scope is controlled at ± 1 hour, in each concrete technology of selecting, each point for measuring temperature temperature accuracy is controlled at ± 0.1 ℃:
Temperature rise period
T
1: first temperature in vitellarium begins to be room temperature, rises to 100 ℃ in 6 hours, rises to 250 ℃ in 14 hours, this moment, constant temperature was 6 hours, rose to 320 ℃ in 10 hours, rose to 330 ℃ in 6 hours, rise to 332 ℃ in 10 hours, slowly heating up at last reached 335 ℃ of crystallisation stage temperature in 20 hours;
T
2: second temperature in vitellarium begins to be room temperature, rises to 105 ℃ in 6 hours, rises to 255 ℃ in 14 hours, this moment, constant temperature was 6 hours, rose to 325 ℃ in 10 hours, rose to 332 ℃ in 6 hours, rise to 334 ℃ in 10 hours, slowly heating up at last reached 337 ℃ of crystallisation stage temperature in 20 hours;
T
3: first temperature of dissolve area begins to be room temperature, rises to 120 ℃ in 6 hours, rises to 270 ℃ in 14 hours, this moment, constant temperature was 6 hours, rose to 340 ℃ in 10 hours, rose to 350 ℃ in 6 hours, rise to 360 ℃ in 10 hours, slowly heating up at last reached 365 ℃ of crystallisation stage temperature in 20 hours;
T
4: second temperature of dissolve area begins to be room temperature, rises to 120 ℃ in 6 hours, rises to 270 ℃ in 14 hours, this moment, constant temperature was 6 hours, rose to 340 ℃ in 10 hours, rose to 350 ℃ in 6 hours, rise to 360 ℃ in 10 hours, slowly heating up at last reached 367 ℃ of crystallisation stage temperature in 20 hours;
T
5Dissolve area thirdly temperature begins to be room temperature, rises to 120 ℃ in 6 hours, rises to 275 ℃ in 14 hours, this moment, constant temperature was 6 hours, rose to 345 ℃ in 10 hours, rose to 355 ℃ in 6 hours, rise to 365 ℃ in 10 hours, slowly heating up at last reached 369 ℃ of crystallisation stage temperature in 20 hours;
Crystallisation stage
T
1: first of vitellarium is 335 ℃, constant temperature 80 days;
T
2: second of vitellarium is 337 ℃, and constant temperature 10 days rose to 338 ℃ in 20 days, rose to 339 ℃ in 20 days, rose to 340 ℃ in 20 days, and constant temperature is 10 days again;
T
3: first of dissolve area is 365 ℃, rises to 366 ℃ in 10 days, rises to 368 ℃ in 20 days, rises to 370 ℃ in 20 days, rises to 372 ℃ in 20 days, rises to 373 ℃ in 10 days;
T
4: second of dissolve area is 367 ℃, rises to 368 ℃ in 10 days, rises to 372 ℃ in 20 days, rises to 376 ℃ in 20 days, rises to 380 ℃ in 20 days, rises to 383 ℃ in 10 days;
T
5: dissolve area thirdly is 369 ℃, rises to 370 ℃ in 10 days, rises to 374 ℃ in 20 days, rises to 378 ℃ in 20 days, rises to 382 ℃ in 20 days, rises to 385 ℃ in 10 days;
At crystallisation stage T on each time period
2With T
1Temperature head be controlled at 2-5 ℃, T
3With T
2Temperature head be controlled at 28-33 ℃, T
4With T
3Temperature head be controlled at 2-10 ℃, T
5With T
4Temperature head be controlled at 2 ℃;
E, autoclave internal pressure slowly rise to 160MPa at crystallisation stage, and finally are controlled at 160 ± 10MPa.
The present invention since selected the arteries and veins reason for the optical-level quartz crystal of A level as seed crystal, simultaneously owing to adopted the alternating temperature measure, thereby guaranteed the arteries and veins reason index of quartz crystal product at crystallisation stage, greatly reduced the probability that acupuncture occurs; The present invention has been also owing to determined the component and the equivalent concentration of suitable growth media, thereby guaranteed Q value, the crystal transparency quality index of product; The present invention has been also owing to determined compactedness in the suitable still, temperature, time and the pressure parameter of autoclave heating, thereby guaranteed the total quality of optical-level quartz crystal product.Adopt the optical-level quartz crystal product percent of pass of explained hereafter of the present invention to reach 98.8%.
The present invention since at crystallisation stage with T
2With T
1The temperature difference of point is controlled at 2-5 ℃, thereby the crystal growth size is even about making in the still; Also since at crystallisation stage with T
3With T
2The point the temperature difference be controlled at 28-33 ℃, thereby make crystal growth before, during and after phase speed be consistent, Q value stabilization, optics are evenly good; Also because T
4With T
3The temperature difference of point is controlled at 2-10 ℃, thereby the degree of supersaturation in crystal growth mid-term, later stage is guaranteed.
The every technical indicator of product all reaches or is better than the prescribed value of GB7895-87, its index: more than the arteries and veins reason index A level; Corrusion tunnel density:＜10/cm
2Q value 〉=3.0 * 10
6Inclusion: more than the Ia class; Optical homogeneity: Δ n≤5 * 10
-6Spectral transmittance when wavelength is 800-2500nm＞95%.The low rotten filter element that utilizes this optical-level quartz crystal material to make is used in digital camera, every technical indicator was stable when PC was used on CCD camera and the television telephone set with CCD camera, system of supervision.
Description of drawings
Accompanying drawing is the process flow sheet of optical-level quartz crystal temperature-variable temperature difference method growth technique of the present invention, and the invention will be further described below in conjunction with accompanying drawing.
Embodiment
Accompanying drawing shows the technical process of optical-level quartz crystal temperature-variable temperature difference method growth technique of the present invention.
One, the preparatory stage
Seed crystal is the crystal seed of synthetic quartzcrystal, at first will be according to the size processing seed crystal of crystal growth.Seed screening arteries and veins reason itself has adopted the high precision multi-cutting machine for A level, inclusion are that the above crystal of Ia class processes on the working method, subsidiary material silicon carbide is the 600-800 order, and rotating speed is 80-100 time/minute.Seed orientation: Y piece seed wafer Z direction thickness is 1.8 ± 0.2mm, and surperficial parallelism reaches 0.05mm, and corrusion tunnel density is less than 10/cm
2
Seed crystal cleans: will cut directed good seed crystal and put into basin and deoil with the detergent immersion cleaning earlier, clean with Ultrasonic Cleaners again and deoil, clear water washes down again, the seed crystal that washes down is put into plastic tub, this is leaked basin place 38-42% hydrofluoric acid solution corrosion 2-3 hour, expose fresh at the small jog of seed crystal face.From hydrofluoric acid solution, take out the leakage basin and place clear water to clean, with the alkaline solution neutralization, clean with ionized water at last again, take out the seed crystal dry for standby then.
Feedstock production: the natural quartz fragment of cultivating quartz crystal is a smelting quartz, adopt transparency greater than 95%, SiO
2Be not less than 99.8%, the granularity path length is the natural stone diamond stone raw material of 2 ± 0.5cm, choose 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, and adds small amount of alkali, can take out raw material in 30 ± 5 minutes from Ultrasonic Cleaners, cross 2 times with deionized water again after cleaning with flowing water, the raw material of the deionized water crossed is inserted dry for standby in the drying baker.
Deionized water preparation: natural water is carried out purification process, make deionized water, its electric conductivity＜3.0 * 10
-6/ ohmcm.
The growth media preparation: it is that 1.2 ± 0.1mol/L, additive adopt LiOHH that main liquid adopts NaOH equivalent concentration
2O, NaNO
2Equivalent concentration is 0.07 ± 0.01mol/L.
The cleaning of former charging basket, iron plate, seed crystal frame, plate washer:
Former charging basket, iron plate are clean with clear water and washed with de-ionized water with emery cloth polishing back earlier.
The seed crystal frame is all clean with pure water and washed with de-ionized water with emery cloth polishing back at every turn.
Plate washer and seed crystal frame are one, and perforate is arranged on plate washer.
The cleaning of autoclave, seed crystal frame, plate washer:
Clean the still inwall three times or wash away the still inwall with high pressure water with clear water, wire 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.
Seed crystal hangs:
Seed wafer is suspended on the seed crystal frame, and every is left mobile space for liquid all around.
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.
Two, the dress still stage
The smelting quartz raw material of cleaning, dry is taken by weighing weight pour in the former charging basket, charging basket is hung in the autoclave.
The solution for preparing is poured in the still.
Clean seed crystal on seed crystal frame and the frame with pure water, put into still then.
Measure the height of liquid level, make the interior compactedness of its still satisfy V to the still mouth
Liquid=(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 volumeThe % of) * (83-84).
Sealing plug is hung in the still mouth, check its planeness.
Big gland is screwed in kettle, and hand push clashes into the end tension of putting forth one's strength in addition of big spanner with sledgehammer or weight after tight again, in order to avoid resilience, clashes into big spanner and rotates the gland angle and be about 60-90 ° and get final product.Reach and make wear ring outer ring and kettle sealing.
On sealing plug, screw in and carry the plug ring flange, mention sealing plug to interior sealing station.
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.
The pressure measuring system device is installed.
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.
Point for measuring temperature T is set from top to bottom in the vitellarium
1And T
2, point for measuring temperature T is set from top to bottom at dissolve area
3, T
4And T
5
Three, the temperature rise period:
T
1: first temperature in vitellarium begins to be room temperature, be generally 30 ℃, in 6 hours, rise to 100 ℃, in 14 hours, rise to 250 ℃, this moment, constant temperature was 6 hours, rose to 320 ℃ in 10 hours, rose to 330 ℃ in 6 hours, rise to 332 ℃ in 10 hours, slowly heating up at last reached 335 ℃ of crystallisation stage temperature in 20 hours.
T
2: second temperature in vitellarium begins to be room temperature, be generally 32 ℃, in 6 hours, rise to 105 ℃, in 14 hours, rise to 255 ℃, this moment, constant temperature was 6 hours, rose to 325 ℃ in 10 hours, rose to 332 ℃ in 6 hours, rise to 334 ℃ in 10 hours, slowly heating up at last reached 337 ℃ of crystallisation stage temperature in 20 hours.
T
3: first temperature of dissolve area begins to be room temperature, be generally 37 ℃, in 6 hours, rise to 120 ℃, in 14 hours, rise to 270 ℃, this moment, constant temperature was 6 hours, rose to 340 ℃ in 10 hours, rose to 350 ℃ in 6 hours, rise to 360 ℃ in 10 hours, slowly heating up at last reached 365 ℃ of crystallisation stage temperature in 20 hours.
T
4: second temperature of dissolve area begins to be room temperature, be generally 40 ℃, in 6 hours, rise to 120 ℃, in 14 hours, rise to 270 ℃, this moment, constant temperature was 6 hours, rose to 340 ℃ in 10 hours, rose to 350 ℃ in 6 hours, rise to 360 ℃ in 10 hours, slowly heating up at last reached 367 ℃ of crystallisation stage temperature in 20 hours.
T
5Dissolve area thirdly temperature begins to be room temperature, be generally 42 ℃, in 6 hours, rise to 120 ℃, in 14 hours, rise to 275 ℃, this moment, constant temperature was 6 hours, rose to 345 ℃ in 10 hours, rose to 355 ℃ in 6 hours, rise to 365 ℃ in 10 hours, slowly heating up at last reached 369 ℃ of crystallisation stage temperature in 20 hours.
The temperature rise period temperature range is controlled at ± and 3 ℃, the time parameter scope is controlled at ± 1 hour, and in each concrete technology of selecting, each point for measuring temperature temperature accuracy is controlled at ± and 0.1 ℃.
Four, crystallisation stage:
T
1: first of vitellarium is 335 ℃, constant temperature 80 days.
T
2: second of vitellarium is 337 ℃, and constant temperature 10 days rose to 338 ℃ in 20 days, rose to 339 in 20 days, rose to 340 ℃ in 20 days, and constant temperature is 10 days again.
T
3: first of dissolve area is 365 ℃, rises to 366 ℃ in 10 days, rises to 368 ℃ in 20 days, rises to 370 ℃ in 20 days, rises to 372 ℃ in 20 days, rises to 373 ℃ in 10 days.
T
4: second of dissolve area is 367 ℃, rises to 368 ℃ in 10 days, rises to 372 ℃ in 20 days, rises to 376 ℃ in 20 days, rises to 380 ℃ in 20 days, rises to 383 ℃ in 10 days.
T
5: dissolve area thirdly is 369 ℃, rises to 370 ℃ in 10 days, rises to 374 ℃ in 20 days, rises to 378 ℃ in 20 days, rises to 382 ℃ in 20 days, rises to 385 ℃ in 10 days.
At crystallisation stage T on each time period
2With T
1Temperature head be controlled at 2-5 ℃, T
3With T
2Temperature head be controlled at 28-33 ℃, T
4With T
3Temperature head be controlled at 2-10 ℃, T
5With T
4Temperature head be controlled at 2 ℃.
The temperature and time parameter of crystallisation stage, wherein temperature range be controlled at ± 3 ℃, the time parameter scope is controlled at ± 1 hour, in each concrete technology of selecting, each point for measuring temperature temperature accuracy is controlled at ± 0.1 ℃.
The autoclave internal pressure slowly rises to 160MPa at crystallisation stage, and finally is controlled at 160 ± 10MPa.
Five, temperature-fall period:
Behind the crystal growth end cycle, adopt slowly cooling, reduce to room temperature reaching 160-170 hour.
Six, unload still and get crystalline substance:
Wait that the crystal growth week after date that arrives design has a power failure cooling naturally.
When the temperature on the kettle is reduced to 70-80 ℃, at each screw thread mouth place apply oil of kettle upper end, so that open autoclave.
The most suitable still of opening took off pressure tester when the temperature on the kettle was reduced to 40-50 ℃.
When driving still, unclamp 8 earlier and carry the plug screw, take out and carry the plug dish.
Sealing plug is squeezed in the kettle, sealing plug and wear ring are broken away from, allow ring shrink and eliminate radial pressure.
Put big spanner on the big gland, hit out big gland, screw out the 2-3 button then with sledgehammer or weight.
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.
Rotate big gland extraction of closure plug, big tamponade, sealing cover, carry a cover system device such as plug dish.
Take out crystal and place 50-60 ℃, clean crystal in the warm water.
Quality inspection, classification, the check of branch specification are put in storage respectively with the crystal after cleaning.
Claims (1)
1. optical-level quartz crystal temperature-variable temperature difference method growth technique, at first clean seed crystal, quartzite raw material, preparation deionized water and growth media, drain with ionized water cleaning autoclave and with surge pump, in cleaned still, put into the former charging basket that quartzite is housed then, inject growth media that has prepared and the seed crystal frame that hangs with seed crystal, measured liquid level, the still mouth is sealed, restart temperature controlling system, the heating high-pressure still is adjusted temperature, pressure, time parameter to the autoclave of sealing, make the quartz crystal growth shaping, it is characterized in that:
A, seed crystal select optical-level quartz crystal arteries and veins reason to be the A level;
B, growth media are that NaOH and the equivalent concentration of 1.2 ± 0.1mol/L is the LiOHH of 0.07 ± 0.01mol/L by equivalent concentration
2O, NaNO
2Form;
Compactedness satisfies V in c, the still
Liquid=(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 volumeThe % of) * (83-84);
D, autoclave heating:
Point for measuring temperature T is set from top to bottom in the vitellarium
1And T
2, point for measuring temperature T is set from top to bottom at dissolve area
3, T
4And T
5, the temperature and time parameter control scope in autoclave when heating, wherein temperature range be controlled at ± 3 ℃, the time parameter scope is controlled at ± 1 hour, in each concrete technology of selecting, each point for measuring temperature temperature accuracy is controlled at ± 0.1 ℃:
Temperature rise period
T
1: first temperature in vitellarium begins to be room temperature, rises to 100 ℃ in 6 hours, rises to 250 ℃ in 14 hours, this moment, constant temperature was 6 hours, rose to 320 ℃ in 10 hours, rose to 330 ℃ in 6 hours, rise to 332 ℃ in 10 hours, slowly heating up at last reached 335 ℃ of crystallisation stage temperature in 20 hours;
T
2: second temperature in vitellarium begins to be room temperature, rises to 105 ℃ in 6 hours, rises to 255 ℃ in 14 hours, this moment, constant temperature was 6 hours, rose to 325 ℃ in 10 hours, rose to 332 ℃ in 6 hours, rise to 334 ℃ in 10 hours, slowly heating up at last reached 337 ℃ of crystallisation stage temperature in 20 hours;
T
3: first temperature of dissolve area begins to be room temperature, rises to 120 ℃ in 6 hours, rises to 270 ℃ in 14 hours, this moment, constant temperature was 6 hours, rose to 340 ℃ in 10 hours, rose to 350 ℃ in 6 hours, rise to 360 ℃ in 10 hours, slowly heating up at last reached 365 ℃ of crystallisation stage temperature in 20 hours;
T
4: second temperature of dissolve area begins to be room temperature, rises to 120 ℃ in 6 hours, rises to 270 ℃ in 14 hours, this moment, constant temperature was 6 hours, rose to 340 ℃ in 10 hours, rose to 350 ℃ in 6 hours, rise to 360 ℃ in 10 hours, slowly heating up at last reached 367 ℃ of crystallisation stage temperature in 20 hours;
T
5Dissolve area thirdly temperature begins to be room temperature, rises to 120 ℃ in 6 hours, rises to 275 ℃ in 14 hours, this moment, constant temperature was 6 hours, rose to 345 ℃ in 10 hours, rose to 355 ℃ in 6 hours, rise to 365 ℃ in 10 hours, slowly heating up at last reached 369 ℃ of crystallisation stage temperature in 20 hours;
Crystallisation stage
T
1: first of vitellarium is 335 ℃, constant temperature 80 days;
T
2: second of vitellarium is 337 ℃, and constant temperature 10 days rose to 338 ℃ in 20 days, rose to 339 ℃ in 20 days, rose to 340 ℃ in 20 days, and constant temperature is 10 days again;
T
3: first of dissolve area is 365 ℃, rises to 366 ℃ in 10 days, rises to 368 ℃ in 20 days, rises to 370 ℃ in 20 days, rises to 372 ℃ in 20 days, rises to 373 ℃ in 10 days;
T
4: second of dissolve area is 367 ℃, rises to 368 ℃ in 10 days, rises to 372 ℃ in 20 days, rises to 376 ℃ in 20 days, rises to 380 ℃ in 20 days, rises to 383 ℃ in 10 days;
T
5: dissolve area thirdly is 369 ℃, rises to 370 ℃ in 10 days, rises to 374 ℃ in 20 days, rises to 378 ℃ in 20 days, rises to 382 ℃ in 20 days, rises to 385 ℃ in 10 days;
At crystallisation stage T on each time period
2With T
1Temperature head be controlled at 2-5 ℃, T
3With T
2Temperature head be controlled at 28-33 ℃, T
4With T
3Temperature head be controlled at 2-10 ℃, T
5With T
4Temperature head be controlled at 2 ℃;
E, autoclave internal pressure slowly rise to 160MPa at crystallisation stage, and finally are controlled at 160 ± 10MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100160202A CN101319375B (en) | 2008-05-08 | 2008-05-08 | Optical-level quartz crystal temperature-variable temperature difference method growth technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100160202A CN101319375B (en) | 2008-05-08 | 2008-05-08 | Optical-level quartz crystal temperature-variable temperature difference method growth technique |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101319375A CN101319375A (en) | 2008-12-10 |
| CN101319375B true CN101319375B (en) | 2010-09-22 |
Family
ID=40179630
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100160202A Expired - Fee Related CN101319375B (en) | 2008-05-08 | 2008-05-08 | Optical-level quartz crystal temperature-variable temperature difference method growth technique |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101319375B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101514490B (en) * | 2009-02-19 | 2011-10-26 | 北京石晶光电科技股份有限公司济源分公司 | Cultivation growing process for optical quartz crystal |
| CN103938271A (en) * | 2014-04-29 | 2014-07-23 | 三明市港乐水晶电子有限公司 | Growth method of piezo-quartz |
| 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 |
| CN106917142A (en) * | 2017-03-14 | 2017-07-04 | 浙江博达光电有限公司 | The growing method of high purity quartz crystal |
| CN109112629A (en) * | 2018-09-06 | 2019-01-01 | 浙江博达光电有限公司 | Single side grows quartz crystal and its growing method |
| CN109137074A (en) * | 2018-10-23 | 2019-01-04 | 梁维嘉 | The artificial culture growing method of quartzy embryo |
| 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 |
| CN115744920A (en) * | 2022-12-13 | 2023-03-07 | 中材人工晶体研究院(山东)有限公司 | Hydrothermal synthesis method of high-purity quartz |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3832146A (en) * | 1972-06-16 | 1974-08-27 | E Bresnahan | High pressure hydrothermal growth of quartz with high "q" values |
| CN1414145A (en) * | 2002-07-17 | 2003-04-30 | 刘盛浦 | Growing technology of optical grade low corrusion tunnel density quartz crystal |
| JP2005015316A (en) * | 2003-06-30 | 2005-01-20 | Kyocera Kinseki Corp | Method of growing artificial quartz crystal |
| CN1865525A (en) * | 2005-05-20 | 2006-11-22 | 淄博宇峰实业有限责任公司 | Method for preparing large-size artificial optical quartz crystal by hydrothermal method |
-
2008
- 2008-05-08 CN CN2008100160202A patent/CN101319375B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3832146A (en) * | 1972-06-16 | 1974-08-27 | E Bresnahan | High pressure hydrothermal growth of quartz with high "q" values |
| CN1414145A (en) * | 2002-07-17 | 2003-04-30 | 刘盛浦 | Growing technology of optical grade low corrusion tunnel density quartz crystal |
| JP2005015316A (en) * | 2003-06-30 | 2005-01-20 | Kyocera Kinseki Corp | Method of growing artificial quartz crystal |
| CN1865525A (en) * | 2005-05-20 | 2006-11-22 | 淄博宇峰实业有限责任公司 | Method for preparing large-size artificial optical quartz crystal by hydrothermal method |
Non-Patent Citations (2)
| Title |
|---|
| 姜付义等.耐辐射优质石英晶体的生长.《人工晶体学报》.2006,第35卷(第3期),666-668. * |
| 韩建儒等.低腐蚀隧道密度压电石英晶体.《山东大学学报(自然科学版)》.2000,第35卷(第1期),69-73. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101319375A (en) | 2008-12-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101319374B (en) | Optical-level single-sided long quartz crystal growth technique | |
| CN101319375B (en) | Optical-level quartz crystal temperature-variable temperature difference method growth technique | |
| CN102412172B (en) | Cut/ground silicon wafer surface cleaning method | |
| CN101805930B (en) | Method for cleaning polyphenylene sulfide melt spinning spinneret | |
| CN102962226A (en) | Method for cleaning polished sapphire substrate wafer | |
| CN102412173B (en) | Cut/ground silicon wafer surface cleaning apparatus | |
| WO2014101261A1 (en) | Method for producing ultra-clean wiping cloth | |
| CN1207447C (en) | Growing technology of optical grade low corrusion tunnel density quartz crystal | |
| CN216749927U (en) | Rework processing system for defective heterojunction battery products | |
| CN104009122A (en) | Processing method for reworking silicon wafers in silk-screen printing | |
| CN102502652A (en) | Cleaning process for polycrystalline material | |
| CN109527900A (en) | A kind of hydrophobic Cotton Weaving by and preparation method thereof | |
| CN101613885B (en) | ZnGeP2 crystal corrosive and corrosion method | |
| CN110643441B (en) | Screen surface cleaning process for liquid crystal screen production | |
| CN109821810A (en) | A kind of sapphire substrate sheet finished product cleaning process | |
| CN104028503B (en) | The cleaning method of silicon material | |
| CN109371456B (en) | Etching device and etching method for artificial quartz crystal seed wafer | |
| CN210386715U (en) | Polycrystalline silicon cleaning device | |
| Talebpour et al. | Degumming of silk yarn using alkali, enzyme and seidlitzia rosmarinus | |
| CN213855985U (en) | Semiconductor wafer dust removal cleaning machine | |
| CN103659468B (en) | A kind of reduce monocrystalline silicon wafer crystal polished silicon wafer chemical burn have wax polishing method | |
| CN112635301A (en) | Method for improving poor back sealing liquid medicine of 8-inch polished wafer | |
| CN107413690A (en) | A kind of Sapphire wafer surface cleaning device and method for different roughness and size | |
| CN112111790A (en) | Artificial wafer corrosion cleaning process | |
| CN211486847U (en) | Polyvinyl alcohol stoste metal filter element belt cleaning device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100922 Termination date: 20140508 |