CN110747502B - High-quality seed crystal piece cultivation method for artificial quartz crystal - Google Patents
High-quality seed crystal piece cultivation method for artificial quartz crystal Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
- B28D5/04—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
- B28D5/04—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools
- B28D5/042—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools by cutting with blades or wires mounted in a reciprocating frame
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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Abstract
The invention discloses a method for cultivating high-quality seed crystal of artificial quartz crystal, which comprises the following steps: firstly, cutting an artificial quartz crystal to be cut into a frame crystal only reserving partial positive and negative electric axis areas; secondly, cutting the frame crystal into frame seed wafers; thirdly, placing the frame seed wafer in a high-pressure kettle for crystal growth; and fourthly, cutting the grown part of the frame crystal to obtain the high-quality seed crystal plate. The invention utilizes the characteristic that the crystal growing in the + X direction (positive electric axis direction) of the quartz crystal can not inherit the defect on the seed wafer to cultivate the high-quality seed wafer, and cuts the grown crystal into the seed wafer, thereby obtaining the high-quality seed wafer with low corrosion tunnel density.
Description
Technical Field
The invention relates to a high-quality seed crystal wafer cultivation process of an artificial quartz crystal, in particular to a frame-shaped + X-direction (positive electric axis direction) crystal growth and seed crystal wafer manufacturing technology of the artificial quartz crystal.
Background
The artificial quartz crystal has good piezoelectric and optical properties and is an important crystal material in the electronic and optical fields.
The artificial quartz crystal grows on the seed crystal by adopting a hydrothermal temperature difference method, the earliest seed crystal is formed by cutting the seed crystal from a natural quartz crystal, the seed crystal of the high-quality quartz crystal is more and more difficult to obtain from the nature along with the exhaustion of the mineral reserves of the high-quality natural quartz crystal, and the existing seed crystal is formed by cutting the artificial quartz crystal; however, due to the crystallization characteristics of the artificial quartz crystal, the defects on the seed crystal wafer are inherited into the grown crystal, and as the seed crystal wafer is continuously cut from the grown artificial quartz crystal, the lattice defects and the corrosion tunnel defects in the seed crystal wafer are more and more accumulated, so that the search for manufacturing the high-quality seed crystal wafer becomes an important research topic in the industry.
In the crystal growth process of the artificial quartz crystal by the hydrothermal temperature difference method, alkaline aqueous solution dissolved with silicon dioxide is convected to a low-temperature zone hung with a seed wafer to form supersaturated silicon dioxide to form crystallization growth on the surface of the seed wafer, according to the crystallization rule of the quartz crystal, the Z direction (optical axis direction) of the seed crystal is a main growth surface, the growth speed is fastest, the defect in the optical axis direction can be inherited to the grown crystal, and the +/-X direction (positive and negative electric axis directions) of the seed crystal also has certain growth.
The technical principle of the frame seed method is explained and confirmed in the document "New TECHNIQUE TO DECREASE DISLOCATION IN SYNTHETIC QUARTZ CRYSTAL", which however does not describe the specific processing of the frame seed wafer; therefore, how to operate to realize the high-quality seed crystal for cultivating the artificial quartz crystal is not known at present.
Disclosure of Invention
The invention aims to provide a high-quality seed crystal cultivation method for artificial quartz crystals.
In order to solve the technical problems, the invention provides a high-quality seed crystal cultivation method of an artificial quartz crystal, which comprises the following steps:
firstly, cutting an artificial quartz crystal to be cut into a frame crystal only reserving partial positive and negative electric axis areas;
secondly, cutting the frame crystal into a frame seed wafer, wherein the thickness of the frame seed wafer is generally 1-2 mm;
thirdly, placing the frame seed wafer in a high-pressure kettle for crystal growth;
and fourthly, cutting the grown part of the frame crystal to obtain a high-quality seed wafer (a low-defect high-quality seed wafer).
As an improvement of the high-quality seed crystal cultivation method of the artificial quartz crystal, the first step is as follows:
grinding the + X surface (positive axial surface) and a Z surface (optical axial surface) of the artificial quartz crystal to be cut to ensure that the orientation precision of the two ground planes is within +/-10'; the cut-out portion (1) is drawn on the other non-ground Z-plane (optical axis plane) and then cut.
Description of the drawings: the temperature of the cut part must be ensured not to exceed 573 ℃ in the cutting process;
drawing the width of the X area to be reserved according to different growing hills and area boundaries of the Z area and the X area on the unground Z surface (optical axis surface); the length direction of the cut-out portion 1 is the longest Y (mechanical axis) length within the crystal framework structure.
As a further improvement of the high-quality seed crystal cultivation method of the artificial quartz crystal, the second step is to sequentially carry out the following steps:
2.1, making a notch of a frame crystal downward, putting the cut part (1) in the step 1) back to the original position of the crystal, pouring a binder (such as a rosin paraffin solution) into a cutting gap, adhering the frame crystal to the cut part (1) and then adhering the frame crystal to a seed crystal cutting iron plate, enabling a negative electric shaft-X part of the frame crystal to be upward and aligning to a frame-shaped metal knife rest of a multi-knife cutting machine, and arranging a cutting knife strip on the frame-shaped metal knife rest;
2.2, carrying out parallelism inspection on the frame-shaped metal tool rest and the seed crystal cutting iron plate so as to enable the movement error to be less than or equal to 0.05 mm; aiming at ensuring the parallelism of the cutting knife strip and the cut crystal;
2.3, preparing cutting fluid for the multi-knife cutting machine;
2.4, cutting the crystal by using a multi-cutter cutting machine under the coordination of cutting liquid, wherein the cutting speed is once to and fro every 4 seconds;
2.5, after the cutting knife strip of the multi-knife cutting machine cuts into the crystal (2 +/-0.2) mm, improving the cutting rate of the multi-knife cutting machine, and enabling the cutting rate to go and go once every 2 seconds; until the frame crystal is cut through;
description of the drawings: after the frame seed crystal is cut through, reducing the running speed of the multi-cutter cutting machine to stop, closing the cutting liquid pump and the hydraulic pump, and lowering the seed crystal cutting iron plate stuck with quartz crystal;
2.6, putting the seed crystal cutting iron plate with the cut frame seed crystals into a sodium hydroxide solution for heating and soaking;
description of the drawings: the sodium hydroxide solution is added for soaking to remove heavy oil dirt of the cutting fluid, and the heating is used for melting the binder and the like;
and 2.7, cleaning the obtained seed crystal to remove oil stains (which can be realized by adopting conventional washing powder and detergent), and removing the embedded part in the middle of the seed crystal to obtain the door-shaped frame seed crystal wafer.
As a further improvement of the method for cultivating the high-quality seed crystal of the artificial quartz crystal,
in the step 2.1, the adhesive is prepared from rosin: paraffin wax is 1:1 in mass ratio;
in the step 2.3, the 320-mesh green silicon carbide abrasive and the grinding cutting oil are mixed according to the weight ratio of 0.8:1 to obtain the cutting fluid.
Description of the drawings: in step 2.1, the crystal is stuck on a seed crystal cutting iron plate, and HM306 quartz crystal special glue can be selected.
As a further improvement of the method for cultivating the high-quality seed crystal of the artificial quartz crystal,
in the step 2.6, each kilogram of water is added with (250 +/-25) grams of NaOH to obtain a sodium hydroxide solution;
heating to boiling and preserving heat for 30 +/-5 minutes so as to realize soaking.
As a further improvement of the high-quality seed crystal cultivation method of the artificial quartz crystal, the third step is as follows:
the frame seed wafer is first subjected to supersaturated NH as an etching solution4HF2Soaking and corroding (3 +/-0.5) hours in an ammonium bifluoride solution, washing with water and drying; then putting the quartz crystal into a high-pressure kettle, and carrying out crystal growth according to a hydrothermal temperature difference method of the artificial quartz crystal; a framework crystal was obtained.
As a further improvement of the high-quality seed crystal cultivation method of the artificial quartz crystal, the fourth step is:
4.1, cutting the frame crystal growing part 6 obtained in the third step like the first step;
4.2, adhering the frame crystal growing part 6 obtained by cutting in the step 4.1 on a seed crystal cutting iron plate, wherein the-X (negative electric axis) part is upward and is aligned with a cutting tool bar of a multi-tool cutting machine;
then, operating according to 2.2-2.6;
and cleaning the cut seed crystal pieces to remove oil stains (which can be realized by adopting conventional washing powder and detergent) to obtain the high-quality seed crystal piece of the artificial quartz crystal.
The length of the seed wafer to be cut is generally 200 to 300 mm.
The grown part of the frame crystal obtained by the invention is subjected to corrosion tunnel density test according to the specification of 4.2.8 in GB/T3352-2012 artificial quartz crystal specification and use guide; can be less than grade Ia specified in the Standard 4.1.5; 3 strips per square centimeter are achieved; and can therefore be referred to as a quality seed wafer.
The method comprises the specific steps of firstly cutting the artificial quartz crystal into a frame-shaped crystal only retaining part of positive and negative electric axis regions, then cutting the frame crystal into a frame seed wafer, then hanging the frame seed wafer into an autoclave for crystal growth, and cutting the part in the frame grown into the crystal again to obtain the high-quality seed wafer with low defects.
The invention relates to a method for manufacturing a high-quality seed wafer by adopting a frame crystal cultivation method. The invention discovers that: the growth direction in the + X direction (positive electric axis direction) is perpendicular to the optical axis direction, defects on the seed crystal are not inherited into the grown crystal, but the growth rate is slower than that in the Z direction (optical axis direction) and that in the-X direction (negative electric axis direction). The invention utilizes the characteristic that the crystal growing in the + X direction (positive electric axis direction) of the quartz crystal can not inherit the defects on the seed wafer to cultivate the high-quality seed wafer, and the grown crystal is subjected to seed wafer cutting to obtain the high-quality seed wafer with low corrosion tunnel density.
The invention utilizes an ultrahigh pressure (300-. Therefore, by adopting the method of the invention, the surface flatness of the cut seed crystal can reach 0.01-0.02 mm; the perpendicularity with the X surface can reach 90 degrees +/-10'.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a schematic view of an artificial quartz crystal.
FIG. 2 is a schematic axial view of a cut frame crystal.
Fig. 3 is a schematic view of a frame crystal after cutting is completed.
Fig. 4 is a schematic view of a frame crystal cutting seed.
Fig. 5 is a schematic view of a frame seed wafer after dicing and punching.
Fig. 6 is a schematic view of the suspension of the frame seed wafer on the seed holder.
Fig. 7 is a schematic view of a frame seed wafer grown crystal.
FIG. 8 shows a high-quality block of crystal obtained by cutting the + X (positive axis direction) extension 6 of the crystal of FIG. 7.
Fig. 9 shows a high quality seed wafer obtained by slicing the high quality crystal block 6 of fig. 8.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
examples 1,
Firstly, cutting the artificial quartz crystal into a frame-shaped crystal (cutting the frame crystal) only keeping partial positive and negative electric axis regions:
an artificial quartz crystal to be cut (as described in figure 1), the crystal length (Y) being about 230 mm; the crystal thickness (Z) is about 75 mm; the crystal width (X) is about 100 mm.
Grinding a Z surface (optical axis surface) and a + X surface (positive axis surface) of an artificial quartz crystal (shown in figure 1) to be cut, wherein the orientation precision of the ground two planes is guaranteed to be within +/-10'; drawing a part to be cut-off-a cut-off part 1 on the other non-grinding Z surface (optical axis surface), namely drawing the width of an X area to be reserved according to different growing hills and area boundary lines of the Z area and the X area on the non-grinding Z surface (optical axis surface) according to the common knowledge in the industry; the length direction of the cut-out portion 1 is the longest Y (mechanical axis) length within the crystal framework structure. And adjusting the cutting speed to control the cutting precision within +/-0.15 mm.
FIG. 1 is a typical quartz crystal shape, wherein the dashed lines are frame crystal cut scribe lines, removed by cut-away portions 1, resulting in a frame crystal, as shown in FIG. 3.
Crystal length (Y)230 mm; crystal thickness (Z)75 mm; the crystal width (X) was 20 mm.
Because the quartz crystal has a phase transformation point from alpha phase to beta phase, the temperature of the cut part must be ensured not to exceed 573 ℃ in the process of carrying out the quartz crystal profile cutting, otherwise, the quartz crystal is cracked due to phase transformation. The cutting of the frame quartz crystal is carried out by using the ultrahigh pressure (300-. Thereby ensuring that no broken edge and jagged edge generated by cutting generate twins and cracks in the crystal growth.
Secondly, cutting the frame crystal into frame seed wafers, and sequentially carrying out the following steps:
2.1, as shown in fig. 3, a notch of the frame crystal is downward, the cut part 1 in the step 1) is placed back to the original position of the crystal, a rosin paraffin solution with the proportion of 1:1 (mass ratio) is poured into a cutting gap, after the rosin paraffin solution is solidified for 2 hours, the crystal is adhered to a seed crystal cutting iron plate by using HM306 quartz crystal special glue, and the-X (negative electric axis) part of the frame crystal is upward and is aligned to a cutting blade of a frame-shaped metal knife rest of a multi-blade cutting machine.
Description of the drawings: a plurality of cutting knife strips (the number of the knife strips is determined according to the width of the knife rest of the multi-knife cutting machine and the cutting thickness of the seed crystal) are separated by a gasket with the thickness of 1-2 mm, and the knife rest of the multi-knife cutting machine is fixed and tensioned;
the cut part 1 of the frame crystal is put back to the original position of the crystal, the main function of the crystal is a filling function, the cutting knife strip in the subsequent step is ensured to uniformly cut the whole crystal material, the cutting liquid can infiltrate into the cutting knife gap, and the phenomenon that the slicing is not uniform due to the shortage of mortar caused by the vacancy in the middle is avoided.
2.2, using a dial indicator to carry out parallelism detection on the frame-shaped metal tool rest and the seed crystal cutting iron plate, so that the movement error is within +/-0.05 mm; the purpose is to ensure the parallelism of the cutting knife strip and the cut crystal.
2.3, preparing cutting fluid (cutting fluid) for the multi-knife cutting machine, mixing 320 # green silicon carbide abrasive with grinding cutting oil according to the weight ratio of 0.8:1, and uniformly stirring by using a stirring pump.
The abrasive cutting oil can be, for example, JX-8 type abrasive cutting oil produced by petroleum chemical research and design institute of Shaanxi province.
2.4, the cutting fluid pump and the multi-blade cutter are started and adjusted to the rate of one round trip every 4 seconds to cut the crystal, see fig. 4.
Description of the drawings: the frame-shaped metal tool rest makes reciprocating linear motion along the length direction (Y direction) of the seed crystal wafer to be cut, under the action of the hydraulic pump, the crystal adhered on the seed crystal cutting iron plate is jacked towards the moving tool rest, and the cutting tool bar cuts (grinds) the quartz crystal under the matching action of cutting liquid (cutting liquid). The thickness of the spacer of the cutting blade is the thickness of the wafer to be cut, and the thickness is generally 1 to 2 mm.
The specific cutting fluid is adopted, so that firstly, the cooling effect is realized, and the quartz crystal is prevented from phase change cracking caused by the temperature rise of a cutting part in the cutting process; and secondly, the green silicon carbide abrasive is conveyed to the cutting surfaces of the cutter bar and the crystal, so that the abrasive is ensured to rub between the cutter bar and the crystal in the linear reciprocating motion of the cutter bar to achieve the cutting effect, and the mixed liquid of the abrasive and the cutting oil flowing down after cutting is pumped back by the cutting liquid pump for recycling.
And 2.5, after the cutting knife strip of the multi-knife cutting machine cuts into the crystal by 2mm, improving the cutting speed of the multi-knife cutting machine to achieve the purpose of reciprocating every 2 seconds.
And after the frame seed crystal is cut completely, reducing the running speed of the multi-cutter cutting machine to stop, and closing the cutting liquid pump and the hydraulic pump to ensure that the seed crystal cutting iron plate stuck with the quartz crystal is lowered.
2.6, taking down the seed crystal cutting iron plate with the cut frame seed crystal, putting the plate into a container, filling tap water (so as to ensure that the cut frame seed crystal is soaked in the water), adding 250 g of NaOH (sodium hydroxide) into each kilogram of water, heating to boil, preserving the heat for 30 minutes, and naturally cooling to room temperature.
Note: the purpose of adding the sodium hydroxide solution for soaking is to remove heavy oil pollution of the cutting fluid, and the heating function is to melt the glue special for HM306 quartz crystals and the rosin paraffin solution.
And 2.7, cleaning the cut seed crystal wafer to remove oil stains (which can be realized by adopting conventional washing powder and detergent), and removing the embedded part in the middle of the seed crystal wafer to obtain the frame seed crystal wafer 2 in the shape of the Chinese character 'men'.
That is, the frame seed wafer 2 is composed of a bottom bar (in the length direction) and beams at both ends of the bottom bar, and the seed wafer is in a gate shape.
Thirdly, placing the frame seed wafer into a high-pressure kettle for crystal growth, and sequentially carrying out the following steps:
3.1, punching 4 holes 3 with phi of 1.5mm at the cross beams at two ends of the frame seed wafer 2 obtained in the step two by using an ultrasonic punching machine; to be used for binding the seed crystal. As shown in fig. 5.
3.2 placing the perforated frame seed wafer 2 in a conventional plastic etch basket and immersing in supersaturated NH at 30 deg.C4HF2(ammonium bifluoride) etching solution; corroding for 3 hours in a well ventilated environment, fishing out and cleaning with clear water; when the PH value of the cleaning liquid generated by cleaning is neutral, putting the seed wafer into an ultrasonic cleaning machine, and continuously cleaning the seed wafer for 20 minutes by using deionized water; and drying the cleaned seed crystal by using a blower for later use.
3.3, penetrating stainless steel wires 4 into seed crystal fixing holes 3 on each frame seed wafer 2; and fixed on the upper and lower frame rings 5 of the seed crystal frame; and the notch direction of the frame seed wafer 2 is kept consistent. As shown in fig. 6.
3.4, putting the seed crystal frame bound with the frame seed crystal wafer 2 into a high-pressure kettle; growing the crystal according to the traditional hydrothermal temperature difference method process of the artificial quartz crystal; for example, the temperature-varying temperature-difference growth process for optical-grade quartz crystals can be performed as 200810016020.2.
3.5, obtaining a frame crystal after the growth period is finished, and obtaining a frame crystal as shown in figure 7; the length (Y) of the crystal is 230mm, and the crystal is grown from a frame seed wafer obtained after crystal growth and kettle opening; crystal thickness (Z)75 mm; the crystal width (X) was 70 mm.
Wherein the frame crystal-grown portion 6 grown from the frame seed wafer in the + X direction (positive electric axis direction) is a portion where an etching tunnel and other seed crystal defects are minimized, i.e., a high-quality crystal portion.
Fourthly, cutting the growing part of the frame crystal, and sequentially carrying out the following steps:
4.1, cutting the frame crystal growing part 6 as the step one;
4.2, gluing a frame crystal growing part 6 (shown in figure 8) obtained by cutting in the step 4.1 on the seed crystal cutting iron plate by using HM306 quartz crystal special glue, wherein the-X (negative electric axis) part is upward and is aligned with a cutting knife strip of the multi-knife cutting machine;
then, operating according to 2.2-2.6;
and cleaning the cut seed crystal pieces to remove oil stains (which can be realized by adopting conventional washing powder and detergent) to obtain the high-quality seed crystal piece of the artificial quartz crystal (figure 9). None of the co-cut 112 pieces produced a crack, nor did they show a significant knife mark.
The surface flatness of the cut seed crystal sheet can reach 0.01-0.02mm through multi-point detection of a dial indicator.
Description of the drawings: carrying out corrosion tunnel density test on the frame crystal growing part 6 obtained by cutting in the step 4.1 according to the specification of 4.2.8 in the national standard GB/T3352-2012 Artificial Quartz Crystal Specification and instruction for use; less than ia specified in this standard 4.1.5; 3 strips per square centimeter are reached.
Comparative example 1, the cutting precision in the first step of example 1 is changed from +/-0.15 mm to +/-0.25 mm, the rest is equal to example 1, and the finally obtained frame crystal growing part 6 has obvious twins; when the seed crystal is cut, 112 pieces of the seed crystal are cut together, and 10 cracks are generated and account for about 8.9 percent of the total number of the slices.
Comparative example 2, the proportion of the rosin paraffin in the second step of example 1 was changed from 1:1 to 0.5:1, and the rest was the same as example 1, which resulted in the filling and frame portion dropping off during the frame crystal cutting.
If the rosin paraffin ratio is changed from 1:1 to 1.5:1, and the rest is the same as that of example 1, the separation of the later mosaic from the frame part is difficult.
Therefore, it is not recommended.
Comparative example 3, the movement error in the parallelism test of step 2.2 of example 1 is changed from +/-0.05 mm to +/-0.1 mm; the rest is equivalent to embodiment 1. The orientation error of the finally obtained seed crystal wafer causes the thickness of the crystals grown on two sides of the seed crystal wafer to be different, the orientation deviation correction of the growing part of the frame crystal is increased, and the number of the seed crystals which can be cut by the frame crystal is reduced.
That is, only 108 pieces could be obtained by cutting, and the number was reduced by 4 pieces compared to 112 pieces of example 1.
Comparative example 4, the weight ratio of the 320-mesh green silicon carbide abrasive and the grinding and cutting oil in step 2.3 of example 1 is changed from 0.8:1 to 1:1, and the rest is identical to example 1.
After the seed crystal slices are cut, 5 obvious cutting knife marks are generated, and account for 4.5 percent of the total number of the slices.
Comparative example 5, the weight ratio of the 320-mesh green silicon carbide abrasive and the grinding and cutting oil in step 2.3 of example 1 is changed from 0.8:1 to 0.5:1, and the rest is equal to example 1.
Resulting in 25 pieces of broken seed pieces accounting for 22.7% of the total pieces during cutting.
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. Such as various directional suspension growth of the seed crystal in a frame and single-sided long suspension and growth, all variations directly derivable or suggested by those skilled in the art from the present disclosure are to be considered within the scope of the present invention.
Claims (6)
1. The high-quality seed crystal cultivating method for artificial quartz crystal includes the following steps:
firstly, cutting an artificial quartz crystal to be cut into a frame crystal only reserving partial positive and negative electric axis areas;
secondly, cutting the frame crystal into frame seed wafers;
the following steps are carried out in sequence:
2.1, making a notch of the frame crystal downward, putting the cut part (1) in the step 1) back to the original position of the crystal, pouring a binder into a cutting gap, adhering the frame crystal to the cut part (1) and then adhering the frame crystal to a seed crystal cutting iron plate, enabling a-X part of the frame crystal to be upward and aligning to a frame-shaped metal knife rest of a multi-knife cutting machine, and arranging a cutting knife strip on the frame-shaped metal knife rest;
2.2, carrying out parallelism inspection on the frame-shaped metal tool rest and the seed crystal cutting iron plate so as to enable the movement error to be less than or equal to 0.05 mm; aiming at ensuring the parallelism of the cutting knife strip and the cut crystal;
2.3, preparing cutting fluid for the multi-knife cutting machine;
2.4, cutting the crystal by using a multi-cutter cutting machine under the coordination of cutting liquid, wherein the cutting speed is once to and fro every 4 seconds;
2.5, after the cutting knife strip of the multi-knife cutting machine cuts into the crystal (2 +/-0.2) mm, improving the cutting rate of the multi-knife cutting machine, and enabling the cutting rate to go and go once every 2 seconds; until the frame crystal is cut through;
2.6, putting the seed crystal cutting iron plate with the cut frame seed crystals into a sodium hydroxide solution for heating and soaking;
2.7, cleaning the obtained seed crystal to remove oil stains, and then removing the embedded part in the middle of the seed crystal to obtain a door-shaped frame seed crystal wafer (2);
thirdly, placing the frame seed wafer in a high-pressure kettle for crystal growth;
and fourthly, cutting the grown part of the frame crystal to obtain the high-quality seed crystal plate.
2. A method for growing a high-quality seed crystal of an artificial quartz crystal according to claim 1, wherein said first step is:
grinding the + X surface and the Z surface of the artificial quartz crystal to be cut to ensure that the orientation precision of the two ground planes is within +/-10'; the cut-out portion (1) is drawn on the other non-ground Z-plane and then cut.
3. A method for growing a high-quality seed crystal of an artificial quartz crystal according to claim 1 or 2, wherein:
in the step 2.1, the adhesive is prepared from rosin: paraffin wax is 1:1 in mass ratio;
in the step 2.3, the 320-mesh green silicon carbide abrasive and the grinding cutting oil are mixed according to the weight ratio of 0.8:1 to obtain the cutting fluid.
4. A method for growing a good-quality seed crystal of an artificial quartz crystal according to claim 3, wherein:
in the step 2.6, each kilogram of water is added with (250 +/-25) grams of NaOH to obtain a sodium hydroxide solution;
heating to boiling and preserving heat for 30 +/-5 minutes so as to realize soaking.
5. A method for growing a high-quality seed crystal of an artificial quartz crystal according to claim 3, wherein said third step is:
the frame seed wafer (2) is first subjected to supersaturated NH as an etching solution4HF2Soaking and corroding (3 +/-0.5) hours in an ammonium bifluoride solution, washing with water and drying; then putting the quartz crystal into a high-pressure kettle, and carrying out crystal growth according to a hydrothermal temperature difference method of the artificial quartz crystal; a framework crystal was obtained.
6. A method for growing a good-quality seed crystal of an artificial quartz crystal according to claim 3, wherein said fourth step is:
4.1, cutting the grown part (6) of the frame crystal obtained in the step three according to the step one;
4.2, adhering the growing part (6) of the frame crystal obtained by cutting in the step 4.1 on a seed crystal cutting iron plate, wherein the part-X is upward and is aligned with a cutting tool bar of the multi-tool cutting machine;
then, operating according to 2.2-2.6;
and cleaning the cut seed crystal pieces, and removing oil stains to obtain the high-quality seed crystal piece of the artificial quartz crystal.
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| JPS5761931A (en) * | 1980-10-01 | 1982-04-14 | Shinkosha:Kk | Knife for microtome and ultra-microtome made of natural of artificial quartz |
| CN101514490A (en) * | 2009-02-19 | 2009-08-26 | 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 |
| CN101603202A (en) * | 2009-05-11 | 2009-12-16 | 北京石晶光电科技股份有限公司 | A kind of seed crystal working method that can present the quartz crystal characteristic structure and shape |
| CN208368475U (en) * | 2018-05-31 | 2019-01-11 | 浙江罗克光电科技有限公司 | A kind of Multi-knife machine precisely cut for chip |
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|---|---|---|---|---|
| JPS5761931A (en) * | 1980-10-01 | 1982-04-14 | Shinkosha:Kk | Knife for microtome and ultra-microtome made of natural of artificial quartz |
| CN101514490A (en) * | 2009-02-19 | 2009-08-26 | 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 |
| CN101603202A (en) * | 2009-05-11 | 2009-12-16 | 北京石晶光电科技股份有限公司 | A kind of seed crystal working method that can present the quartz crystal characteristic structure and shape |
| CN208368475U (en) * | 2018-05-31 | 2019-01-11 | 浙江罗克光电科技有限公司 | A kind of Multi-knife machine precisely cut for chip |
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