CN103938271A - Growth method of piezo-quartz - Google Patents
Growth method of piezo-quartz Download PDFInfo
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- CN103938271A CN103938271A CN201410176925.1A CN201410176925A CN103938271A CN 103938271 A CN103938271 A CN 103938271A CN 201410176925 A CN201410176925 A CN 201410176925A CN 103938271 A CN103938271 A CN 103938271A
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Abstract
The invention discloses a growth method of piezo-quartz. The method comprises the steps of performing cleaning preparation on raw materials; performing cleaning preparation on a high-pressure kettle and auxiliary components in the kettle; heating for 29 hours according to the following temperature-time relationships: (1) the interval time of heating started after the kettle is arranged is less than 4 hours; (2) the temperature of the upper part of the kettle is controlled to be 100 DEG C, the temperature of the lower part of the kettle is controlled to be 115 DEG C at the same time, and the time length of the time period is set to be 6 hours; (3) the temperature of the upper part of the kettle is controlled to be 250 DEG C, the temperature of the lower part of the kettle is controlled to be 275 DEG C, and the time length of the time period is set to be 14 hours; (4) the temperature of the upper part of the kettle is controlled to be 345-348 DEG C, the temperature of the lower part of the kettle is controlled to be 375-376 DEG C, and the time length of the time period is set to be 9 hours; heating for 29 hours, then preserving heat for 65 days according to given curves of the temperature-time relationships, then naturally cooling to a temperature lower than 100 DEG C, and opening the high-pressure kettle. Because the details such as the time-temperature curves and the like are optimized, the growth method is relatively more complete in process and more ideal in use effect.
Description
Technical field
The invention belongs to synthetic quartz manufacturing technology field, relate to a kind of growth method of piezoelectric quartz.
Background technology
Synthetic quartz growth is the general hydrothermal temperature difference method that adopts at present, in the autoclave of vertical sealed, carries out.In autoclave, quartzy particle is placed as nutrilite (this part is called dissolve area) by the about 2/5-1/2 in bottom place.Place seed crystal frame at 3/5-1/2 place, this top, the seed crystal of certain cut type that on frame, suspension growth crystal is used, this district is called vitellarium.Between vitellarium and dissolve area, have a baffle plate with certain percentage of open area, this baffle plate can make the two interval certain temperature difference (certainly, being also subject to indirect heating power influences) that form, so that the upper and lower convection current of solution.In autoclave, pack into and there is certain density alkaline aqueous solution, be generally sodium hydroxide or sodium carbonate, and design certain packing density, after sealing, heat, produce the pressure of 135-150MPa, because the temperature of dissolve area, autoclave bottom is than the temperature of top vitellarium high (by the power control of heating system), general high approximately 30 DEG C of left and right, so produce the convection current of solution in still, when the quartzy particle of dissolve area is along with the temperature of alkaline solution raises, solubleness increases gradually, the state until reach capacity, due under, the temperature difference on top and solution convection current, the solution of dissolve silica is brought to still internal upper part vitellarium by baffle plate, because the temperature of vitellarium is lower than dissolve area (approximately 30 DEG C), now, Si02 in the solution state that reaches capacity, and on the seed crystal of vitellarium, carry out crystallization, recrystallization, seed crystal is constantly grown up, now because the dilute solution after convection action crystallization is back to dissolve area, again dissolve smelting quartz material, so move in circles and make crystal continue to grow up, can control growth size thickness and the gross weight of crystal by design requirements, stop heating to certain hour, after naturally cooling, open the synthetic quartz crystal that still takes out growth.
Piezoelectric quartz refers to the synthetic quartz with piezoelectric effect.Can be made into quartz resonator, ultrasonic generator, wave filter and various load-sensing units etc. with it.Be widely used in radio industry, national defense industry.Very strict to the specification of quality of piezoelectric quartz.Piezoelectric quartz must be the monocrystalline of complete crystallization, can not contain the flaws such as inclusion, crack, plethora, can not be twin crystal.Therefore, the growth of piezoelectric quartz requires higher, also has some special processing requirements in the time adopting above hydrothermal temperature difference method.
For obtaining artificial piezoelectric quartz in batches, people have explored the batch production growth method of some piezoelectric quartzes.
For example: publication number is CN101275273, a kind of manufacture method of piezoelectric quartz is disclosed in the Chinese patent of " a kind of manufacture method of piezoelectric quartz " by name, its step is as follows: choose particulate state natural quartz masonry and cultivate body, be fed into autoclave bottom after cleaning; In autoclave, add high purity water; Upper and lower seed crystal frame is packed in autoclave, and seed crystal is suspended on respectively on upper and lower seed crystal frame, on upper and lower seed crystal frame, be fixed with upper, middle and lower division board simultaneously, on described upper, middle and lower division board, be equipped with convection holes; Sealing autoclave; Start autoclave, keeping autoclave internal upper part temperature is that 340-345 DEG C, middle part temperature are that 370-380 DEG C, temperature of lower are 380-385 DEG C; Keeping autoclave internal pressure is 115-150MPa, until piezoelectric quartz ordered crystalline completes in autoclave.The inventive method is simple, workable, can make that Q value is greater than 3,600,000, corrusion tunnel density is less than 50/cm
3, zero inclusion piezoelectric quartz.
Adopt the growth method of the piezoelectric quartz of above technology certainly can use, but have the following disadvantages: this technique only provides loading method, temperature, these main processing parameters of pressure, but the process of growth of artificial piezoelectric quartz is a complicated process, except loading method, temperature, outside these main Parameter Conditions of pressure, time, heating curve, a lot of details such as how convection holes arranges all can have a significant impact the quality of the piezoelectric quartz generating, therefore, the growth method of the piezoelectric quartz of prior art is perfect not enough comparatively speaking, result of use is desirable not enough.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides one relatively more perfect, result of use is the growth method of piezoelectric quartz more preferably.
The present invention for the technical scheme that reaches above-mentioned technical purpose and adopt is: a kind of growth method of piezoelectric quartz, and its step is as follows:
A, choose particulate state natural quartz masonry cultivate body, quartzite is placed in to washing powder and soaks 20-24h completely, after taking out, water rinses, and the quartzite that contains accompanying impurities and epidermis ore is removed simultaneously, use again deionized water rinsing one time, cleaned quartzite is fed into autoclave bottom; The loading height of quartzite in autoclave is lower than the lower group of residing position height of heating member; In autoclave, add high purity water;
B, the seed wafer having openning hole is placed in to diluted hydrofluoric acid soaks 4-6h, the surface contamination irony that seed wafer is produced in cutting, punching process washes, then be placed in Ultrasonic Cleaners by clean the dirt removal of plane of crystal, seed crystal is suspended on seed crystal frame, on seed crystal frame, be fixed with division board, division board is provided with convection holes simultaneously; Before dress still, autoclave inner-wall, seed crystal frame, bracing frame, division board are cleaned and remove protective membrane and greasy dirt with alkaline solution, the residual graphite paper on the embryo on still mouth and trim is cleaned up, seed crystal frame is packed in autoclave into sealing autoclave;
C, intensification, adopt temperature program(me) control device automatically to control autoclave and heat up, and keeping autoclave internal pressure is 115-150MPa, and the relation between temperature and time is set to:
(1), still is less than 4h after installing to the interval time that starts to heat up;
(2), the control of still upper temp is 100 DEG C, still temperature of lower control is simultaneously 115 DEG C, this time period duration is set to 6h;
(3), the control of still upper temp is 250 DEG C, the control of still temperature of lower is 275 DEG C, this time period duration is set to 14h;
(4), the control of still upper temp is 345-348 DEG C, the control of still temperature of lower is 375-376 DEG C, this time period duration is set to 9h;
D, insulation, after intensification balance, the control of still upper temp is 345-348 DEG C, the control of still temperature of lower is 375-376 DEG C, adopts temperature program(me) control device automatically to control autoclave insulation 65 days, within the time of 65 days, the top and the bottom temperature difference is adjusted into 42-44 DEG C gradually; In the process of the adjustment top and the bottom temperature difference, the variation of reference pressure, if pressure is toward rising, so just turns down still upper temp, allows Tc toward declining; If pressure, toward declining, is so just heightened still temperature of lower, allow solvent temperature toward rising; Later stage can be reduced still top and the bottom temperature according to altering moderate pressure situation simultaneously;
E, insulation stop insulation after 65 days, by temperature in the kettle be naturally down to 100 DEG C following after, machine oil (adding a little diesel oil) is poured into the screw thread place of autoclave, open autoclave.
Described autoclave is that internal diameter is the round shape autoclave of 250 millimeters, and the circular baffle plate body in autoclave chamber is located at the middle part of autoclave inner chamber and coaxial with autoclave, offers the convection holes that is no less than on circular baffle plate body; Described convection holes comprises the round center hole that arranges with baffle plate body concentric, along six uniform holes of circle of the uniform setting of baffle plate body central angle; The diameter of circular baffle plate body is 247 millimeters; The diameter of round center hole is 33 millimeters; The distance in the center of circle of the center of circle in uniform hole and circular baffle plate body is 36 millimeters; The diameter in circular uniform hole is 12 millimeters.
The invention has the beneficial effects as follows: because the present invention is except providing the underlying condition of loading method, temperature, these main parameters of pressure, also optimize while providing a lot of detail conditions such as m-heating curve, technique is relatively more perfect, and result of use is better.
Embodiment
Embodiments of the invention are as follows:
A growth method for piezoelectric quartz, its step is as follows:
A, choose particulate state natural quartz masonry cultivate body, quartzite is placed in to washing powder and soaks 20-24h completely, after taking out, water rinses, and the quartzite that contains accompanying impurities and epidermis ore is removed simultaneously, use again deionized water rinsing one time, cleaned quartzite is fed into autoclave bottom; The loading height of quartzite in autoclave is lower than the lower group of residing position height of heating member; In autoclave, add high purity water;
B, the seed wafer having openning hole is placed in to diluted hydrofluoric acid soaks 4-6h, the surface contamination irony that seed wafer is produced in cutting, punching process washes, then be placed in Ultrasonic Cleaners by clean the dirt removal of plane of crystal, seed crystal is suspended on seed crystal frame, on seed crystal frame, be fixed with division board, division board is provided with convection holes simultaneously; Before dress still, autoclave inner-wall, seed crystal frame, bracing frame, division board are cleaned and remove protective membrane and greasy dirt with alkaline solution, the residual graphite paper on the embryo on still mouth and trim is cleaned up, seed crystal frame is packed in autoclave into sealing autoclave;
C, intensification, keeping autoclave internal pressure is 115-150MPa, adopts temperature program(me) control device automatically to control autoclave and heats up, the relation between temperature and time is set to:
(1), still is less than 4h after installing to the interval time that starts to heat up;
(2), the control of still upper temp is 100 DEG C, still temperature of lower control is simultaneously 115 DEG C, this time period duration is set to 6h;
(3), the control of still upper temp is 250 DEG C, the control of still temperature of lower is 275 DEG C, this time period duration is set to 14h;
(4), the control of still upper temp is 345-348 DEG C, the control of still temperature of lower is 375-376 DEG C, this time period duration is set to 9h;
D, insulation, after intensification balance, the control of still upper temp is 345-348 DEG C, the control of still temperature of lower is 375-376 DEG C, adopts temperature program(me) control device automatically to control autoclave insulation 65 days, within the time of 65 days, the top and the bottom temperature difference is adjusted into 42-44 DEG C gradually; In the process of the adjustment top and the bottom temperature difference, the variation of reference pressure, if pressure is toward rising, so just turns down still upper temp, allows Tc toward declining; If pressure, toward declining, is so just heightened still temperature of lower, allow solvent temperature toward rising; Later stage can be reduced still top and the bottom temperature according to altering moderate pressure situation simultaneously;
E, insulation stop insulation after 65 days, by temperature in the kettle be naturally down to 100 DEG C following after, machine oil (adding a little diesel oil) is poured into the screw thread place of autoclave, open autoclave.
Described autoclave is that internal diameter is the round shape autoclave of 250 millimeters, and the circular baffle plate body in autoclave chamber is located at the middle part of autoclave inner chamber and coaxial with autoclave, offers the convection holes that is no less than on circular baffle plate body; Described convection holes comprises the round center hole that arranges with baffle plate body concentric, along six uniform holes of circle of the uniform setting of baffle plate body central angle; The diameter of circular baffle plate body is 247 millimeters; The diameter of round center hole is 33 millimeters; The distance in the center of circle of the center of circle in uniform hole and circular baffle plate body is 36 millimeters; The diameter in circular uniform hole is 12 millimeters.
Other specification specified that note also in the invention process are as follows:
One, the preparation before growth:
Preparation work before growth is the important step of crystal growth, comprising cleaning, the orientation of seed crystal, and the cleaning of quartz, the cleaning of autoclave and seed crystal frame and bracing frame, the calculating of liquid level, inspection and the correction of the inspection of sealing element and thermometric, the system such as heat.
(1), the cleaning of seed crystal, orientation
Its specific practice of the cleaning of seed crystal is first the seed wafer having openning hole to be placed in to diluted hydrofluoric acid to soak 4-6 hour, and the surface contamination irony while its objective is cutting, punching washes.Then be placed in Ultrasonic Cleaners by clean the dirt removal of plane of crystal.
Attention: if the time of soaking is oversize, easily produce corrosion excessive in hydrofluoric acid, cause directed unclear; The solubility of hydrofluoric acid is excessively rare, easily produces corrosion inadequate, cannot be directed.
(2), the cleaning of quartzite
Determine quartzy consumption according to the thickness of autoclave content, seed crystal area and expectation institute growing crystal.The purity (foreign matter content) of quartz directly has influence on the quality of crystal, if do not washed clean clearly equally, will directly have influence on the purity of solution when impurity enters solution.
When cleaning, should first quartz be placed in to washing powder and soak 20-24 hour completely, repeatedly rinse with tap water again, when flushing, the quartz of the mineral ore that contains accompanying impurities and epidermis ore should be chosen, clean up rear for subsequent use, again use deionized water rinsing one time packing into before autoclave, surface dust is cleaned again.
Attention: quartz can not exceed the height of lower group of heating collar (or electric stove wire) at the height of autoclave, if exceed 3-5
cm will produce crust, thereby has influence on upper and lower temperature difference and organize up and down the speed of convection current.
(3), the cleaning of autoclave and seed crystal frame and support
The protective membrane that all forms one deck greyish-green at autoclave still wall and seed crystal frame, bracing frame, baffle surface, its composition is aegirine [NaFe (Si03) 2], this layer of protective membrane can prevent that alkaline solution from corroding autoclave wall.But this layer of protective membrane can increase along with the number of times of growth, can progressive additive.Meeting local shedding in the time reaching certain thickness; this is because autoclave dilation causes; sometimes may be also because autoclave wall is caused by mask pattern, the local collision of bracing frame; what value was proposed attention is that this layer of protective layer is made up of particulate aegirine; so just likely enter crystal in solution, form sheet or granular inclusion in the time scattering after sag of protecting coating.
Before each dress still, the cleaning of still wall and mask pattern etc. is even more important, particularly even more important concerning the autoclave of female thread structure, greasy dirt in internal thread must clean up with alkaline solution, in order to avoid greasy dirt is entered in still, also must clean up the graphite paper on embryo and trim on still mouth.
(4), the calculating of liquid level
For the calculating of packing density, it should be noted that the variation due to season, the height of water temperature can make under same packing density, pressure difference when balance.Safety and growth velocity for crystal growth all can have larger impact.
(5), inspection and the correction of the inspection of sealing element and thermometric, the system such as heat.
1., check whether wear ring is out of shape, and whether the contact surface of trim and autoclave is greater than 2/3rds;
Whether the pad face 2., between meter connector and sealing plug is intact, has or not chipping;
3., whether back to zero of tensimeter, whether table pipe stops up with the through hole of sealing plug;
4., KHY-1B temperature regulator, silicon controlled rectifier, etc. add Thermal Control Element and have or not damage;
5., whether thermopair be that pair using in a upper cycle, has or not damage;
6., heating zone (resistance wire) have or not and burn, whether the insulation at iron sheet head and steel leader tape line outlet place intact;
7., whether clamp bolt is loosening.
Two, dress still and crystal growth
(1), dress still
Before dress still, to check the mated condition of all parts, the particularly autoclave to female thread structure, should note allowing wear ring and the pressure ring relief groove lower than autoclave internal thread, if after exceeding, wear ring and pressure ring stress deformation, thus cause entering relief groove place, bring difficulty not only can to the unlatching of autoclave, even can be out of shape excessively due to pressure ring, cause sealing plug to be difficult to extract, to cause the scratch of still mouth and internal thread damage.
After autoclave installs, should put into immediately still hole, build muffler, insulation quilt (pillow), heat.It should be noted, after still installs to the warming room interval can not oversize (can not exceed 4 hours), because the time one is long, the solid tiny particle that impurity in solution or still wall come off is just easily attached in seed crystal face, in the time of crystal growth, these impurity are just wrapped in crystal, so just on seed crystal interface, form one deck stressor layers, occur splitting along the shellfish of seed face with regard to tending to when opening crystal after still.
(2), intensification, temperature control
When intensification, should strictly control the temperature difference in conjunction with power, lower group temperature must be higher than upper group of temperature, first dissolves with the quartz of guaranteeing bottom, if upper and lower temperature is identical, or upper group during higher than lower group, and seed crystal is just likely melted.
In the process of the adjustment top and the bottom temperature difference, the variation of reference pressure, if pressure is toward rising, so just turns down still upper temp, allows Tc toward declining; If pressure, toward declining, is so just heightened still temperature of lower, allow solvent temperature toward rising; Later stage can be reduced still top and the bottom temperature according to altering moderate pressure situation simultaneously.
Attention: although for bigbore autoclave, thermal capacity is large, the temporal variation of outside temperature at short notice, impact on autoclave is relatively little, it is long that but the time cycle of temperature variation can not continue, after autoclave temp variation is excessive, the inclusion of crystal is just had to obvious impact.So in the process of lifting insulation quilt, the unpredictable factor such as variation, temperature hysteresis of envrionment temperature should be taken into account.
When in process of growth, the temperature difference is larger, crystal growth speed obviously speeds, and simultaneously when excessive temperature differentials, in crystal, inclusion also increases, and cylinder increases, transparency variation.Sometimes in the top crystal in autoclave, on crystal face upward, deposited a large amount of K
+, Na
+siliceous colloid molecule, cooling after because colloid molecule is different from the shrinkage coefficient of crystal, form fried head.
Three, stop still, drive still
After crystal growth end cycle, while stopping still, to note the temperature organized up and down, decline when faster if organize temperature in lower group of temperature suppression ratio, easily form the knot end, so just need inspection heating system and heat-insulation system.
Below temperature is down to 100 degree time, machine oil (adding a little diesel oil) is injected to autoclave screw thread place, object is the oilness increasing between still mouth screw, so that open autoclave.
1., unclamp and take off and carry plug dish open still step:, lay sealing plug; 2., the large spiral shell of outwarding winding, carry plug; 3., take out mask pattern, cut crystal; 4., clean crystal with warm water; 5., clean autoclave mouth and epimere still wall with residual solution; 6., pour out residual solution and residual quartz; 7., clean still chamber with steel brush, and rinse well with deionized water; 8., cover still mouth, hang in dress still hole, prepare dress still.
Attention: thermopair is bound to still number mark meter in the time stopping still, put into fixed position, insulation quilt, insulation pillow, muffler are placed on specified location to use after dress still next time.Before dress still, please first determine next time and completely examine the date next time of this still, to arrange kind, determine growth cycle.
Claims (2)
1. a growth method for piezoelectric quartz, is characterized in that: its step is as follows:
A, choose particulate state natural quartz masonry cultivate body, quartzite is placed in to washing powder and soaks 20-24h completely, after taking out, water rinses, and the quartzite that contains accompanying impurities and epidermis ore is removed simultaneously, use again deionized water rinsing one time, cleaned quartzite is fed into autoclave bottom; The loading height of quartzite in autoclave is lower than the lower group of residing position height of heating member; In autoclave, add high purity water;
B, the seed wafer having openning hole is placed in to diluted hydrofluoric acid soaks 4-6h, the surface contamination irony that seed wafer is produced in cutting, punching process washes, then be placed in Ultrasonic Cleaners by clean the dirt removal of plane of crystal, seed crystal is suspended on seed crystal frame, on seed crystal frame, be fixed with division board, division board is provided with convection holes simultaneously; Before dress still, autoclave inner-wall, seed crystal frame, bracing frame, division board are cleaned and remove protective membrane and greasy dirt with alkaline solution, the residual graphite paper on the embryo on still mouth and trim is cleaned up, seed crystal frame is packed in autoclave into sealing autoclave;
C, intensification, keeping autoclave internal pressure is 115-150MPa, adopts temperature program(me) control device automatically to control autoclave and heats up, the relation between temperature and time is set to:
(1), still is less than 4h after installing to the interval time that starts to heat up;
(2), the control of still upper temp is 100 DEG C, still temperature of lower control is simultaneously 115 DEG C, this time period duration is set to 6h;
(3), the control of still upper temp is 250 DEG C, the control of still temperature of lower is 275 DEG C, this time period duration is set to 14h;
(4), the control of still upper temp is 345-348 DEG C, the control of still temperature of lower is 375-376 DEG C, this time period duration is set to 9h;
D, insulation, after intensification balance, the control of still upper temp is 345-348 DEG C, the control of still temperature of lower is 375-376 DEG C, adopts temperature program(me) control device automatically to control autoclave insulation 65 days, within the time of 65 days, the top and the bottom temperature difference is adjusted into 42-44 DEG C gradually; In the process of the adjustment top and the bottom temperature difference, the variation of reference pressure, if pressure is toward rising, so just turns down still upper temp, allows Tc toward declining; If pressure, toward declining, is so just heightened still temperature of lower, allow solvent temperature toward rising; Later stage can be reduced still top and the bottom temperature according to altering moderate pressure situation simultaneously;
E, insulation stop insulation after 65 days, by temperature in the kettle be naturally down to 100 DEG C following after, machine oil (adding a little diesel oil) is poured into the screw thread place of autoclave, open autoclave.
2. the growth method of a kind of piezoelectric quartz according to claim 1, it is characterized in that: described autoclave is that internal diameter is the round shape autoclave of 250 millimeters, circular baffle plate body in autoclave chamber is located at the middle part of autoclave inner chamber and coaxial with autoclave, offers the convection holes that is no less than on circular baffle plate body; Described convection holes comprises the round center hole that arranges with baffle plate body concentric, along six uniform holes of circle of the uniform setting of baffle plate body central angle; The diameter of circular baffle plate body is 247 millimeters; The diameter of round center hole is 33 millimeters; The distance in the center of circle of the center of circle in uniform hole and circular baffle plate body is 36 millimeters; The diameter in circular uniform hole is 12 millimeters.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104988575A (en) * | 2015-06-25 | 2015-10-21 | 北京石晶光电科技股份有限公司济源分公司 | Reaction kettle and technology used for growing yellow crystals |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323922A (en) * | 2000-05-12 | 2001-11-28 | 索耶研究产品公司 | Method and apparatus for growth of crystal |
| CN101275273A (en) * | 2007-12-25 | 2008-10-01 | 刘运河 | Manufacturing method for piezoelectric quartz |
| CN101319375A (en) * | 2008-05-08 | 2008-12-10 | 刘盛浦 | Optical-level quartz crystal temperature-variable temperature difference method growth technique |
-
2014
- 2014-04-29 CN CN201410176925.1A patent/CN103938271A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323922A (en) * | 2000-05-12 | 2001-11-28 | 索耶研究产品公司 | Method and apparatus for growth of crystal |
| CN101275273A (en) * | 2007-12-25 | 2008-10-01 | 刘运河 | Manufacturing method for piezoelectric quartz |
| CN101319375A (en) * | 2008-05-08 | 2008-12-10 | 刘盛浦 | Optical-level quartz crystal temperature-variable temperature difference method growth technique |
Non-Patent Citations (1)
| Title |
|---|
| 王强涛: "高品质石英晶体生长及性能表征", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104988575A (en) * | 2015-06-25 | 2015-10-21 | 北京石晶光电科技股份有限公司济源分公司 | Reaction kettle and technology used for growing yellow crystals |
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Application publication date: 20140723 |