CN1382842A - Method and equipment for growing monocrystal of cadmium selenide by gas-phase vertical pulling - Google Patents
Method and equipment for growing monocrystal of cadmium selenide by gas-phase vertical pulling Download PDFInfo
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- CN1382842A CN1382842A CN 02113405 CN02113405A CN1382842A CN 1382842 A CN1382842 A CN 1382842A CN 02113405 CN02113405 CN 02113405 CN 02113405 A CN02113405 A CN 02113405A CN 1382842 A CN1382842 A CN 1382842A
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Abstract
A vertical gas-phase pulling-up method for growing cadmium selenide monocrystal features that the cadmium selenide powder is used as raw material and the purification of raw material and the growth of monocrystal are performed in a single ampoul consisting of tubular body divided into purifying and growing segment, heat conducting rod and hanging ring. The said method includes cleaning ampoul, charging raw material, vacuumizing, sealing, multi-stage purifying, cutting and separating ampoul, thermal cleaning growing segment, growing crystal and cooling. The resultant monocrystal features complete structure, high uniformity, low stress, bit size phi(10-20)X(30-40)mm and high resistivity (10 to power 6-8 omega cm).
Description
One, technical field
The invention belongs to the single crystal preparation field, particularly a kind of method of growing monocrystal of cadmium selenide.
Two, background technology
Cadmium selenide (CdSe) single crystal is a kind of II-VI wide bandgap compound semiconductor material, in recent years owing to excellent indoor temperature nucleus radiation detection performance and the non-linear optical property that it had receives much attention, but because the fusing point higher (1239 ℃) of cadmium selenide, two kinds of constituent element vapour pressures that constitute it are bigger, the crystalline thermal conductivity is low, therefore prepares relatively difficulty of large size high-quality monocrystal of cadmium selenide.At present, liquid phase method, thermograde melt zone melting method and static vapor growth method are mainly adopted in the preparation of CdSe single crystal.The weak point of liquid phase method is: the single crystal size of being grown is less, is generally several millimeters, and crystals contains the residual solvent parcel, thereby application is restricted.The weak point of thermograde melt zone melting method is: 1, crystal growth needs high pressure vessel, causes cost to improve, and insecurity increases; 2, the crystal stress that grows is big, and defective is many, and is of low quality.The weak point of static vapor growth method is: 1, crystal leaves standstill growth, causes crystalizing interface to move, and growth temperature ladder is non-constant, and radially warm field distribution is inhomogeneous, thereby influences crystal growth, is difficult to form structural integrity, uniform single crystal; 2, the crystal resistivity that grows is low, generally 10
1～2Ω cm.
Three, summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of method and specific equipment of growing monocrystal of cadmium selenide by gas-phase vertical pulling is provided, big to prepare size, the high-quality monocrystal of cadmium selenide that resistivity is high.
The present invention is a kind of improvement to static vapor growth method, and with respect to static vapor growth method, the present invention is anti-pollution in the removal of impurities of raw material, innovate aspect the processing condition of crystal growth.
Method provided by the invention is a raw material with the cadmium selenide powder, and being grown in the same ampoule of the purification of raw material and single crystal finished, and comprises following processing step successively:
1, cleaning ampoule
The cleaning ampoule is the processing of the ampoule inwall being removed impurity, to reduce the foreign matter content in the crystal;
2, charging and remove the sealing gland small jar
The cadmium selenide powder is packed in the ampoule after the cleaning, the degasification of under 400 ℃～600 ℃, finding time then, to remove the organic impurity in the raw material, the air pressure in ampoule reduces to 10
-3～10
-4Envelope small jar during Pa, and make the cadmium selenide powder be positioned at the ampoule rectifying section;
3, multistage purification
Multistage purification adopts the distillation method of purification to get rid of the high-melting-point inorganic impurity, the temperature of promptly repeatedly ampoule being contained the raw material place is heated to 950 ℃～1050 ℃, cadmium selenide is repeatedly distilled be delivered to the cold zone crystallization, till cadmium selenide is delivered to ampoule growth section from the distillation of ampoule rectifying section, the regional thermograde of purifying maintains 20～30 ℃/centimetre, and the fed distance that at every turn distils is controlled at 5～10 centimetres;
4, cutting and separating ampoule
The cutting and separating ampoule is with oxyhydrogen flame the rectifying section of ampoule to be become two sections with a growth section cutting and separating, and the growth section sealed knot of cadmium selenide will be housed, and makes its inside still keep 10
-3～10
-4The Pa high vacuum state;
5, warm wash growth section
Warm wash growth section is carried out in two regions perpendicular growth furnace, regulate furnace temperature, making the temperature on ampoule growth section top is 1000 ℃～1200 ℃, temperature than its underpart raw material district is high 100 ℃～and 200 ℃, under the effect of temperature difference motivating force, the adsorbed raw material of growth section upper inside wall is thoroughly driven to the lower feed district, has promptly finished the warm wash of growth section;
6, crystal growth and cooling
Be inverted the warm field distribution in the two regions perpendicular growth furnace, make the temperature on ampoule growth section top be lower than the temperature in raw material district, its underpart, the temperature on ampoule growth section top is 1000 ℃～1020 ℃, the temperature in ampoule growth pars infrasegmentalis raw material district is 1080 ℃～1100 ℃, the crystallizing field thermograde is controlled at 6～8 ℃/centimetre, the ampoule rate of pulling is controlled at 3～8 millimeters/day, speed of rotation is controlled at 2～5 rev/mins, can finish the growth of monocrystal of cadmium selenide under these conditions, after single crystal growth is finished, be cooled to room temperature by 20～30 ℃/hour speed and can obtain required monocrystal of cadmium selenide.
For thoroughly removing the impurity of ampoule inwall, avoid the pollution of crystal growth vessel to raw material, " cleaning ampoule " this step in the aforesaid method has adopted comprehensive cleaning and vacuum bakeout process combined:
1, the comprehensive cleaning
At first soak flushing ampoule inwall with tap water, injecting the hydrofluoric acid washing lotion then soaked 3～5 minutes, extremely neutral with the tap water flushing again, also washed repeatedly in 8～10 minutes with cleaned by ultrasonic vibration at last with the high resistant deionized water, remain in the impurity of ampoule inwall with removal;
2, vacuum bakeout
Cleaned ampoule is placed vacuum drying oven, and temperature is controlled at 120 ℃～150 ℃, and the time is 3～4 hours, with the water vapour of thorough removal ampoule inside.
The enforcement of aforesaid method must be disposed corresponding apparatus, except that conventional existing devices such as vacuum drying oven, electric tube furnace, ultrasonic cleaner, also needs the ampoule and the two regions perpendicular growth furnace of design specialized.
Ampoule provided by the invention mainly by blind end be conical tubular body arranged inside, the heat conductive rod that is connected with the tubular body arranged inside conical end and the link that is connected with heat conductive rod form, tubular body arranged inside is separated into rectifying section and growth section by neck, the free end end of rectifying section has charging bole, the conical portion section of growth section end is provided with neck, this neck makes the conical portion section form " jujube nuclear shape " molectron with " horn-like ", help eliminating unnecessary nucleus, bonding nucleus growth.
Better for the purification and the crystalline growth result that make raw material, also adopted following technical scheme during the ampoule design:
1, ampoule rectifying section length is 3～5: 1 with the ratio of growth segment length, i.e. rectifying section length: growth segment length=3～5: 1;
2, the cone angle of ampoule growth section end-cone shape portion section is 25 °～30 °;
Tubular body arranged inside is generally made by quartz, and its caliber determines that according to the diameter of prepared single crystal its length is determined according to the distance of the progression of multistage purification, each distillation conveying and prepared single crystal length.
Two regions perpendicular growth furnace provided by the invention comprise body of heater, are installed in heating unit, temperature measuring equipment and temperature regulating device on the body of heater, heating unit is along the axial distribution of body of heater and connect into two groups of independently heating systems, one group of top heat supply that heating systems is a stove, another group heating systems is the bottom heat supply of stove.
In order to measure furnace temperature exactly and to control furnace temperature effectively, temperature measuring equipment is intensive real-time measurement apparatus, reach the transfer lever and the temperature indicating instrument that are connected with thermopair by the thermopair that is installed in different thermometrics position in the stove more than three groups and form, form up and down by the thermopair and the temperature controller of stove by being positioned at for temperature regulating device.
The present invention has following beneficial effect:
1, prepared monocrystal of cadmium selenide structural integrity, good uniformity, stress are little, and size can reach φ (10～12) * (30～40) millimeter, and the resistivity of the harsh single crystal that grows can reach 10
6～8Ω cm, the resistivity of single crystal can reach 10 after the thermal treatment
9～10Ω cm, thereby wide application are particularly suitable for making indoor temperature nucleus radiation detector.
2, the multistage purification of raw material and single crystal growth phase in same ampoule had both been avoided having simplified growth technique again because of raw material shifts the secondary pollution that causes effectively, had reduced the crystal growth cost.
3, the comprehensive cleaning and the vacuum bakeout process combined of cleaning ampoule can be reduced to minimum level with the impurity in the container, have application value.
4, whole process flow is pollution-free, security good, is easy to control.
5, neck is set and, helps eliminating unnecessary nucleus, bonding nucleus growth, preparation large size single crystal body in ampoule growth section the optimized choice of this section cone angle.
6, two regions perpendicular growth furnace are rational in infrastructure, not only guaranteed the enforcement of method provided by the present invention, and can use in association area.
7, method provided by the invention not only is suitable for the growth of cadmium selenide monocrystal material, can also be applied to the preparation of other II-VI compound semiconductor monocrystalline.
Four, description of drawings
Fig. 1 is the process flow diagram of method provided by the invention;
Fig. 2 is a kind of structure iron of ampoule provided by the invention;
Fig. 3 is the synoptic diagram of the multistage purifying technique step in the method provided by the invention;
The scheme of installation of ampoule growth section when Fig. 4 is a kind of structure diagram of two regions perpendicular growth furnace provided by the invention and warm wash and crystal growth;
Fig. 5 is a kind of X ray diffracting spectrum of the prepared monocrystal of cadmium selenide of method provided by the invention;
Fig. 6 is a kind of dislocation pit figure of the prepared monocrystal of cadmium selenide of method provided by the invention.
Five, embodiment
Embodiment:
The present embodiment preparation size is the monocrystal of cadmium selenide of 10 * 40 millimeters of φ, employed ampoule as shown in Figure 2, quartzy tubular body arranged inside, heat conductive rod 4 and link 5 by 10 millimeters * 600 millimeters of φ are formed, tubular body arranged inside is separated into rectifying section 1 and growth section 2 by neck 3, rectifying section is 3: 1 with the length ratio of growth section, the end of growth section is enclosed construction and is cone, the cone angle of this conical end is 25 °, this conical portion section is provided with neck 6, is beneficial to nucleus and eliminates the growth of formation monokaryon for how much.
The technical process of present embodiment is followed successively by following steps as shown in Figure 1:
1, cleaning ampoule
The cleaning ampoule adopts comprehensive the cleaning and the vacuum bakeout process combined:
(1) the comprehensive cleaning
At first soak flushing ampoule inwall, inject the hydrofluoric acid washing lotion then and soaked 3 minutes with tap water, extremely neutral with the tap water flushing again, place the ultrasonic cleaner vibration to clean 8 minutes and washed repeatedly at last with the high resistant deionized water;
(2) vacuum bakeout
Cleaned ampoule is placed vacuum drying oven, and temperature is controlled at 130 ℃, and storing time is 3.5 hours;
2, charging and remove the sealing gland small jar
The powder 18 that commercially available high purity cadmium selenide polycrystalline is ground to form restrains in the ampoule of packing into after cleaning, the degasification of under 500 ℃, finding time then, and the air pressure in ampoule reduces to 10
-4Envelope small jar during Pa, and make the cadmium selenide powder be positioned at A place, ampoule rectifying section end, as shown in Figure 3.
3, multistage purification
Multistage purification as shown in Figure 3, at first ampoule rectifying section end A is placed several centimeters in the horizontal purification furnace, furnace temperature is risen to 1000 ℃ then, the regional thermograde of purifying maintains 25 ℃/centimetre, distillation for the first time carry be make cadmium selenide to be separated by 8 centimetres the B place cold zone crystallization of A place, after the whole distillations of cadmium selenide are delivered to the crystallization of B place, ampoule is advanced 8 centimetres in stove, so repeatedly, be transported to the growth section E place of ampoule through cadmium selenide raw material after 6 grades of distillation removal of impurities, the high-melting-point inorganic impurity then is left in the rectifying section AC zone of ampoule;
4, cutting and separating ampoule
After multistage purification is finished, ampoule is taken out in stove, it is become two sections from neck D horizontal resection, and the EF growth section sealed knot of cadmium selenide will be housed, make its inside still remain on 10 with oxyhydrogen flame
-4The Pa high vacuum state;
5, warm wash growth section
Warm wash growth section is carried out in two regions perpendicular growth furnace, the structure of this kind stove as shown in Figure 4, comprise body of heater 7, be installed in the heating unit 8 on the body of heater, temperature measuring equipment and temperature regulating device, heating unit 8 is along the body of heater axial distribution and connect into two groups of independently heating systems, one group of top heat supply that heating systems is a stove, another group heating systems is the bottom heat supply of stove, temperature measuring equipment is installed in the PtRh/Pt thermopair 9 at different thermometrics position in the stove by five groups and transfer lever 10 and the temperature indicating instrument 11 that is connected with thermopair formed, and form up and down by the PtRh/Pt thermopair 12 and the REX-P90 precision temperature controller of stove by being positioned at for temperature regulating device.Concrete operations are to make ampoule growth section top (conical end) be positioned at stove top, raw material district, its underpart is positioned at lower furnace, as shown in Figure 4, regulate furnace temperature, the temperature that makes stove top is 1100 ℃, the temperature of lower furnace is 900 ℃, under the effect of temperature difference motivating force, the adsorbed raw material of growth section upper inside wall is thoroughly driven to the lower feed district;
6, crystal growth and cooling
Crystal growth is still carried out in two regions perpendicular stoves, and the mounting means in the ampoule growth Duan Zailu is identical during with warm wash, as shown in Figure 4.The processing condition of crystal growth: the temperature on ampoule growth section top (conical end) is 1020 ℃, the temperature in ampoule growth pars infrasegmentalis raw material district is 1100 ℃, the crystallizing field thermograde is 6 ℃/centimetre, and the ampoule rate of pulling is that 5 millimeters/day, ampoule speed of rotation are 3 rev/mins.Under above-mentioned processing condition, can grow into the monocrystal of cadmium selenide of 10 * 40 millimeters of φ through the time about two weeks, after single crystal growth is finished, be cooled to room temperature by 25 ℃/hour speed and can obtain required monocrystal of cadmium selenide.
The X ray diffracting spectrum of the monocrystal of cadmium selenide that present embodiment is prepared as shown in Figure 5, the dislocation pit as shown in Figure 6, from Fig. 5, Fig. 6 as can be seen, complete, the good uniformity of crystalline structure; After tested, the resistivity of the harsh single crystal that grows is 10
8Ω cm, resistivity after heat treatment is 10
10Ω cm belongs to high resistant fine monocrystal of cadmium selenide material.
Claims (8)
1, a kind of method of growing monocrystal of cadmium selenide by gas-phase vertical pulling is a raw material with the cadmium selenide powder, and being grown in the same ampoule of the purification of raw material and single crystal finished, and comprises following processing step successively:
(1) cleaning ampoule
The cleaning ampoule is the processing of the ampoule inwall being removed impurity;
(2) charging and remove the sealing gland small jar
With the cadmium selenide powder pack into the cleaning after ampoule in, the degasification of under 400 ℃～600 ℃, finding time then, the air pressure in ampoule reduces to 10
-3～10
-4Envelope small jar during Pa, and make the cadmium selenide powder be positioned at the ampoule rectifying section;
(3) multistage purification
Multistage purification adopts the distillation method of purification to get rid of the high-melting-point inorganic impurity, the temperature of promptly repeatedly ampoule being contained the raw material place is heated to 950 ℃～1050 ℃, cadmium selenide is repeatedly distilled be delivered to the cold zone crystallization, till cadmium selenide is delivered to ampoule growth section from the distillation of ampoule rectifying section, the regional thermograde of purifying maintains 20～30 ℃/centimetre, and the fed distance that at every turn distils is controlled at 5～10 centimetres;
(4) cutting and separating ampoule
The cutting and separating ampoule is with oxyhydrogen flame the rectifying section of ampoule to be become two sections with a growth section cutting and separating, and the growth section sealed knot of cadmium selenide will be housed, and makes its inside still keep 10
-3～10
-4The Pa high vacuum state;
(5) warm wash growth section
Warm wash growth section is carried out in two regions perpendicular growth furnace, regulate furnace temperature, making the temperature on ampoule growth section top is 1000 ℃～1200 ℃, temperature than its underpart raw material district is high 100 ℃～and 200 ℃, under the effect of temperature difference motivating force, the adsorbed raw material of growth section upper inside wall is thoroughly driven to the lower feed district, has promptly finished the warm wash of growth section;
(6) crystal growth and cooling
Be inverted the warm field distribution in the two regions perpendicular growth furnace, make the temperature on ampoule growth section top be lower than the temperature in raw material district, its underpart, the temperature on ampoule growth section top is 1000 ℃～1020 ℃, the temperature in ampoule growth pars infrasegmentalis raw material district is 1080 ℃～1100 ℃, the crystallizing field thermograde is controlled at 6～8 ℃/centimetre, the ampoule rate of pulling is controlled at 3～8 millimeters/day, speed of rotation is controlled at 2～5 rev/mins, can finish the growth of monocrystal of cadmium selenide under these conditions, after single crystal growth is finished, be cooled to room temperature by 20～30 ℃/hour speed and can obtain required monocrystal of cadmium selenide.
2, the method for growing monocrystal of cadmium selenide by gas-phase vertical pulling according to claim 1 is characterized in that cleaning ampoule and adopts comprehensive the cleaning and the vacuum bakeout process combined:
(1) the comprehensive cleaning
At first soak and wash the ampoule inwall, inject the hydrofluoric acid washing lotion then and soaked 3～5 minutes with tap water, extremely neutral with the tap water flushing again, also washed repeatedly in 8～10 minutes with cleaned by ultrasonic vibration at last with the high resistant deionized water;
(2) vacuum bakeout
Cleaned ampoule is placed vacuum drying oven, and temperature is controlled at 120 ℃～150 ℃, and the time is 3～4 hours.
3, a kind of for implementing the custom-designed ampoule of the described method of claim 1, comprise that blind end is conical tubular body arranged inside, it is characterized in that also comprising heat conductive rod (4) that is connected with the tubular body arranged inside conical end and the link (5) that is connected with heat conductive rod, tubular body arranged inside is separated into rectifying section (1) and growth section (2) by neck (3), rectifying section free end end has charging bole, the conical portion section of growth section end is provided with neck (6), and this neck makes the conical portion section form " jujube nuclear shape " molectron with " horn-like ".
4, ampoule according to claim 3 is characterized in that the cone angle of the section of growth end-cone shape portion section is 25 °～30 °.
5,, it is characterized in that the rectifying section (1) and the length ratio of growth section (2) are 3～5: 1 according to claim 3 or 4 described ampoules.
6, a kind of for implementing the custom-designed two regions perpendicular growth furnace of the described method of claim 1, comprise body of heater (7), be installed in heating unit (8), temperature measuring equipment and temperature regulating device on the body of heater, it is characterized in that heating unit (8) is along the axial distribution of body of heater and connect into two groups of independently heating systems, one group of top heat supply that heating systems is a stove, another group heating systems is the bottom heat supply of stove.
7, two regions perpendicular growth furnace according to claim 6 is characterized in that temperature measuring equipment reaches the transfer lever (10) and the temperature indicating instrument (11) that are connected with thermopair by the thermopair (9) that is installed in different thermometrics position in the stove more than three groups and forms.
8,, it is characterized in that form up and down by the thermopair (12) and the temperature controller of stove by being positioned at for temperature regulating device according to claim 6 or 7 described two regions perpendicular growth furnace.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021134057A CN1176254C (en) | 2002-02-28 | 2002-02-28 | Method and equipment for growing monocrystal of cadmium selenide by gas-phase vertical pulling |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021134057A CN1176254C (en) | 2002-02-28 | 2002-02-28 | Method and equipment for growing monocrystal of cadmium selenide by gas-phase vertical pulling |
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|---|---|
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| CN1176254C CN1176254C (en) | 2004-11-17 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630881A (en) * | 2015-02-28 | 2015-05-20 | 安庆美晶新材料有限公司 | Method for ultrasonically improving two-dimensional material mono-crystal chemical vapor transportation growth quality |
| CN106498491A (en) * | 2016-11-02 | 2017-03-15 | 中国电子科技集团公司第四十六研究所 | A kind of purifying plant of vapor phase method crystal growth raw material and its method of purification |
| CN108166063A (en) * | 2017-12-26 | 2018-06-15 | 哈尔滨工业大学 | A kind of selenizing Cd monocrystal method of vapor-phase growing of top seed crystal heat conduction |
| CN106477536B (en) * | 2016-10-17 | 2018-10-16 | 西北工业大学 | A kind of preparation method of ultra-high purity cadmium selenide polycrystalline material |
-
2002
- 2002-02-28 CN CNB021134057A patent/CN1176254C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630881A (en) * | 2015-02-28 | 2015-05-20 | 安庆美晶新材料有限公司 | Method for ultrasonically improving two-dimensional material mono-crystal chemical vapor transportation growth quality |
| CN106477536B (en) * | 2016-10-17 | 2018-10-16 | 西北工业大学 | A kind of preparation method of ultra-high purity cadmium selenide polycrystalline material |
| CN106498491A (en) * | 2016-11-02 | 2017-03-15 | 中国电子科技集团公司第四十六研究所 | A kind of purifying plant of vapor phase method crystal growth raw material and its method of purification |
| CN106498491B (en) * | 2016-11-02 | 2018-12-14 | 中国电子科技集团公司第四十六研究所 | A kind of purifying plant and its method of purification of vapor phase method crystal growth raw material |
| CN108166063A (en) * | 2017-12-26 | 2018-06-15 | 哈尔滨工业大学 | A kind of selenizing Cd monocrystal method of vapor-phase growing of top seed crystal heat conduction |
| CN108166063B (en) * | 2017-12-26 | 2019-07-16 | 哈尔滨工业大学 | A kind of selenizing Cd monocrystal method of vapor-phase growing that top seed crystal is thermally conductive |
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| Publication number | Publication date |
|---|---|
| CN1176254C (en) | 2004-11-17 |
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