CN105603394A - Device and method for measuring evaporation quantity of raw material in chemical vapor deposition furnace - Google Patents
Device and method for measuring evaporation quantity of raw material in chemical vapor deposition furnace Download PDFInfo
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- CN105603394A CN105603394A CN201511035099.XA CN201511035099A CN105603394A CN 105603394 A CN105603394 A CN 105603394A CN 201511035099 A CN201511035099 A CN 201511035099A CN 105603394 A CN105603394 A CN 105603394A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
- G01N7/16—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by heating the material
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Abstract
The invention provides a device for measuring the evaporation quantity of a raw material in a chemical vapor deposition furnace. The device comprises a buoyancy device, a shaft filament, a winding device and a meter with a real-time display function. The buoyancy device is arranged on the top of the solid raw material in the chemical vapor deposition furnace and connected with one end of the shaft filament. The other end of the shaft filament is connected with the winding device, and the winding device is fixed above the solid raw material in the chemical vapor deposition furnace. The axis portion of the winding device is connected with the meter with the real-time display function. According to the measuring device, the evaporation quantity of the raw material can be monitored and controlled in real time, and high precision is achieved. Especially, under high-temperature, vacuum and other closed conditions, shaft filament type measurement is adopted, the influence of the temperature on part thermal expansion is lowered, and by means of the connection mode, good safety is achieved in the actual use process, and the requirement of the chemical vapor deposition furnace for high air tightness cannot be affected.
Description
Technical field
The present invention relates to chemical vapour deposition technique field, relate in particular to a kind of dress of measuring raw materials evaporate amountPut and method.
Background technology
Modern science and Technology Need use the New Inorganic Materials of a large amount of Various Functions, and these functional materials mustMust be high-purity, or the dopant material that some kinds impurity forms wittingly in high-purity material. ChangeLearning vapour deposition is the new technology of the preparation inorganic material that grows up nearly decades. Chemical vapour deposition techniqueBe widely used in purifying substances, developed new crystal, the various monocrystalline of deposit, polycrystalline or glassy state inorganic thinMembrane material.
Chemical vapour deposition technique is a kind of method of vapor-phase growing of preparing material, and it is that one or more are containedThere are the compound, the elementary gas that form film element to pass into the reative cell that is placed with base material, by space gasPhase chemistry reaction deposits the technology of solid film on matrix surface. These materials can be oxide,Sulfide, nitride, carbide or selenides can be also two in III-V, II-IV, IV-VI familiesCompound between first or polynary element, and the deposition that their physical function can be by gas phase dopingJourney is accurately controlled. At present, chemical vapour deposition (CVD) has become a frontier of inorganic synthetic chemistry.
Chemical deposition has plurality of advantages, can be under middle temperature or high temperature, by the precursor compound of gaseous stateBetween gas-phase chemical reaction and form solid matter and be deposited on matrix; Can be at normal pressure or vacuum barUnder part; Adopt plasma and laser assisted technology can promote significantly chemical reaction, make the deposition can beAt low temperature, carry out; And the chemical composition of coating can change with the change of gas phase composition, therebyObtain gradient deposition thing or obtain mixing coating, can also control density and the coating purity of coating; EspeciallyBe can be on the matrix of complicated shape and on granular materials plated film, be applicable to applying the work of various complicated shapesPart, good around plating performance due to it, thus can apply with trough, hole, or even the workpiece of blind hole,Can also carry out gas phase disturbance to chemical reaction by various technology, to improve its structure etc.
Utilize at present chemical vapour deposition technique to come, in the process of preparing product, generally to participate in chemical vapour deposition (CVD)A kind of raw material may be solid, all the other raw materials are gas, gas can adopt flowmeter Measurement accuracy gasThe real-time traffic of body, but solid is difficult to measure in real time the amount of its reaction, especially at large-scale chemical gasPhase cvd furnace. Chemical vapor deposition stove is an airtight space, and temperature is higher, more difficult real-timeThe response situation of monitoring the inside solid. Especially in practical application, the real-time production that material quantity is large, ifReacting dose that can not Real-Time Monitoring solid material, also just can not adjust the ratio of each raw material in course of reactionExample, can affect the performance of the deposited product obtaining, and causes a large amount of production wastes.
In addition, in chemical vapor deposition processes, need higher temperature, consider the impact of temperature, andAlso need to consider the problems such as air-tightness and security.
Therefore, how to obtain a kind of Measurement accuracy and can Real-Time Monitoring and the chemical vapour deposition (CVD) of controlThe raw materials evaporate amount of stove is one of focus that production firm and user pay close attention to jointly in the industry always.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of chemical vapor deposition stove of measuringThe apparatus and method of raw materials evaporate amount, measurement assembly provided by the invention can Real-Time Monitoring and is controlled raw materialEvaporation capacity, and the result of the raw materials evaporate amount obtaining has higher accuracy.
The device that the invention provides a kind of raw materials evaporate amount of measuring chemical vapor deposition stove, comprises, floatingPower apparatus, axial filament, coiler device and the meter composition that can show in real time;
Described buoyant device is placed in the solid material top in chemical vapor deposition stove, described buoyant device withOne end of described axial filament is connected;
The other end of described axial filament is connected with described coiler device, and described coiler device is fixed on chemical gasSolid material top in phase cvd furnace;
The axle center of described coiler device is connected with the described meter that can show in real time.
Preferably, described buoyant device is hollow circular cylinder or hollow sphere.
Preferably, the material of described buoyant device is high purity graphite, C/C composite or quartz; Described axleSilk is molybdenum filament, copper wire or tungsten filament.
Preferably, described coiler device is axle core, and the material of described coiler device is identical with axial filament.
Preferably, described meter is rotary encoder.
A kind of method that the invention provides raw materials evaporate amount of measuring chemical vapor deposition stove, comprises followingStep:
A) coiler device in measurement mechanism is fixed on to the solid material top in chemical vapor deposition stove,Buoyant device is placed in the solid material top in chemical vapor deposition stove, and makes axial filament vertically without varicose;
B), while described solid material being all molten into liquid charging stock, described measurement mechanism records initial count;
C) described liquid charging stock is become in the process of steam, described measurement mechanism records the second counting;
D) according to the girth of described initial count, the second counting, coiler device with measure initial count and theThe time difference of two countings, obtain the raw materials evaporate amount in the unit interval.
Preferably, described step D) be specially:
D1) according to described the second counting and the difference of initial count, then be multiplied by the girth of coiler device,Become the coiling length of axial filament in the process of steam to described liquid charging stock;
D2), according to the coiling length of axial filament with hold the cross-sectional area of utensil of described liquid charging stock, obtainBecome the volume of the liquid of steam;
D3) according to the time difference of the initial count of measuring and the second counting, described in become the liquid of steamThe density of volume and described liquid charging stock, obtains raw materials evaporate amount in the unit interval.
The invention provides device or above-mentioned any one skill described in a kind of above-mentioned any one technical schemeMethod described in art scheme is in the application of calculating in solid evaporation capacity.
Preferably, described solid evaporation capacity is specially, a kind of in closed container, high temperature and vacuum orSolid evaporation capacity in multiple situation.
Preferably, the described equipment that need to calculate solid evaporation capacity is chemical vapor deposition stove or single crystal growing furnace.
The device that the invention provides a kind of raw materials evaporate amount of measuring chemical vapor deposition stove, comprises, floatingPower apparatus, axial filament, coiler device and the meter composition that can show in real time; Described being placed in of buoyant deviceLearn the solid material top in gaseous phase deposition stove, described buoyant device is connected with one end of described axial filament;The other end of described axial filament is connected with described coiler device, and it is heavy that described coiler device is fixed on chemical gaseous phaseSolid material top in long-pending stove; The axle center of described coiler device and the described meter phase that can show in real timeConnect. Compared with prior art, measurement mechanism provided by the invention can Real-Time Monitoring and is controlled raw materialEvaporation capacity, has higher accuracy. Especially under the airtight condition such as high temperature, vacuum, the present invention adoptsMeasure by axial filament formula, reduced the impact of temperature on parts thermal expansion, thereby greatly improved certainty of measurement,And connected mode of the present invention, in actual use procedure, there is good security, can shadow yetRing the requirement of chemical vapor deposition stove to high-air-tightness.
Experimental result shows, adopts the raw materials evaporate amount of measurement chemical vapor deposition stove provided by the inventionDevice, the evaporation rate accuracy of measuring raw metal in chemical vapor deposition processes is higher, and deviation existsWithin ± 1.5%.
Brief description of the drawings
The device of the raw materials evaporate amount of the measurement chemical vapor deposition stove that Fig. 1 provides for the embodiment of the present inventionStructural representation sketch.
Detailed description of the invention
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is retouchedState, but should be appreciated that these are described is in order to further illustrate the features and advantages of the present invention, andIt not the restriction to invention claim.
The all raw materials of the present invention, are not particularly limited its source, on market, buy or according to abilityPrepared by the conventional method that field technique personnel know.
The all raw materials of the present invention or parts, be not particularly limited its model, ripe with those skilled in the artThe model of knowing.
The device that the invention provides a kind of raw materials evaporate amount of measuring chemical vapor deposition stove, comprises, floatingPower apparatus, axial filament, coiler device and the meter composition that can show in real time;
Described buoyant device is placed in the solid material top in chemical vapor deposition stove, described buoyant device withOne end of described axial filament is connected;
The other end of described axial filament is connected with described coiler device, and described coiler device is fixed on chemical gasSolid material top in phase cvd furnace;
The axle center of described coiler device is connected with the described meter that can show in real time.
The present invention is not particularly limited described chemical vapor deposition stove, with well known to those skilled in the artChemical vapor deposition stove.
In the present embodiment, the device of the raw materials evaporate amount of described measurement chemical vapor deposition stove (is measured dressPut) in buoyant device contact with the solid material top in chemical vapor deposition stove, its role is to along withThe rising of temperature, solid material becomes liquid state, and buoyant device obtains initial position; Along with the continuation of temperatureRaise, liquid raw material is consumed, and the height of buoyant device can change again, thereby can be real-timeTo the consumption of the interior raw material of stove, thereby be the follow-up solid material in chemical deposition process that detects more exactlyConsumption.
In the present embodiment, described buoyant device is connected with one end of described axial filament, its role is to byThe variation of buoyant device is measured; In other embodiments, buoyant device also can with axial filament arbitrarilyPosition is connected, can accurately embody the preferred version that is changed to of buoyant device.
In the present embodiment, described buoyant device is preferably hollow circular cylinder or hollow sphere, more preferablyHollow circular cylinder, its role is to float on the metal bath surface of molten condition, can be accurately with liquid stateThe height change of raw material and change location; In other embodiments, the diameter of described buoyant device and formThere is no special requirement, those skilled in the art can calculate according to the volume of the density of raw material, liquid charging stockDraw the buoyant device of the volume that meets above-mentioned requirements.
In the present embodiment, the material of described buoyant device is preferably high purity graphite, C/C composite or stoneEnglish, more preferably high purity graphite; In other embodiments, described buoyant device can be also other materials,With stable performance, do not react with other reactants, can not affect the product of chemical vapour deposition (CVD) finished productMatter is preferred version.
In the present embodiment, described axial filament is molybdenum filament, copper wire or tungsten filament, its role is to accurately to countThe change in location of amount buoyant device; In other embodiments, described axial filament can be also other materials, withThermal coefficient of expansion is little, can wire high temperature resistant, that diameter is less be preferred version.
In the present embodiment, the diameter of described axial filament is less than or equal to 0.2mm, its role is to even densityBe wrapped on described coiler device; In other embodiments, the diameter of described axial filament also can carry out itHe selects, taking can even density be wrapped on described coiler device as preferred version.
The other end of axial filament of the present invention is connected with described coiler device, and described coiler device is fixed onSolid material top in chemical vapor deposition stove.
In the present embodiment, described coiler device is preferably fixed on the solid material in chemical vapor deposition stoveTop, its role is to embody accurately the variation relation of axial filament and buoyant device; In other enforcementIn example, described coiler device also can be fixed on other positions, to embody accurately axial filament and buoyant deviceVariation relation be preferred version.
In the present embodiment, described coiler device is axle core or axle sleeve, its role is to facilitate axial filamentBe wound around accurately; In other embodiments, described coiler device can be also other forms, with sideJust axial filament is accurately wound up as preferred version.
In the present embodiment, the material of described coiler device is identical with axial filament, its role is to hot conditionsUnder, can be identical with axial filament thermal expansion; In other embodiments, described coiler device can be also otherMaterial, taking can reduce as far as possible thermal expansion on the impact of Measurement accuracy as preferred version.
The axle center of coiler device of the present invention is connected with the described meter that can show in real time.
In the present embodiment, the axle center of described coiler device is connected with the described meter that can show in real time,Its role is in metering process, the number of turns that on described coiler device, existing axial filament reduces, can pass throughThe meter that can show in real time measures; In other embodiments, other positions of described coiler deviceAlso can be connected with the described meter that can show in real time, can show accurately and measure axial filamentChanging distance is preferred version.
In the present embodiment, described meter is preferably rotary encoder, its role is to accurate recording instituteState the number of turns that on coiler device, existing axial filament reduces; In other embodiments, described meter is also passableFor other equipment that can show in real time, taking the variation distance that can show accurately and measure axial filament for preferredScheme.
The invention provides a kind of device of the raw materials evaporate amount of measuring chemical vapor deposition stove, can be real-timeThe evaporation capacity of monitoring and control raw material, has higher accuracy. Especially airtight in high temperature, vacuum etc.Under condition, the present invention adopts axial filament formula to measure, and has reduced the impact of temperature on parts thermal expansion, thereby largeImprove greatly certainty of measurement, and the parts such as metal axial filament and axle core of the present invention's employing, making of realityHigher with security in process, and connected mode of the present invention, in actual use procedure, can not yetAffect the requirement of chemical vapor deposition stove to high-air-tightness.
The present invention also provides a kind of method of the raw materials evaporate amount of measuring chemical vapor deposition stove, comprise withLower step:
A) coiler device in measurement mechanism is fixed on to the solid material top in chemical vapor deposition stove,Buoyant device is placed in the solid material top in chemical vapor deposition stove, and makes axial filament vertically without varicose;
B), while described solid material being all molten into liquid charging stock, described measurement mechanism records initial count;
C) described liquid charging stock is become in the process of steam, described measurement mechanism records the second counting;
D) according to the girth of described initial count, the second counting, coiler device with measure initial count and theThe time difference of two countings, obtain the raw materials evaporate amount in the unit interval.
It is former that first the present invention is fixed on the coiler device in measurement mechanism solid in chemical vapor deposition stoveMaterial top, buoyant device is placed in the solid material top in chemical vapor deposition stove, and makes the vertical nothing of axial filamentVaricose; On described coiler device, be preferably wound with axial filament. The present invention does not limit especially to above-mentioned steps,Those skilled in the art can adjust according to actual conditions, taking stably measured original state as preferably squareCase.
When the present invention is all molten into liquid charging stock by described solid material subsequently, described measurement mechanism recordsInitial count. The present invention is not particularly limited described solid material, with well known to those skilled in the artThe conventional raw metal that adopts chemical vapour deposition technique, the present invention is preferably metallic zinc.
The present invention becomes described liquid charging stock in the process of steam again, and described measurement mechanism records secondNumber. The process that the present invention becomes steam to described liquid charging stock is not particularly limited, can be for all becomingSteam also can become steam for part. The present invention is also preferably general designation to described the second counting, at thisIn bright, become in the process of steam at aforesaid liquid raw material, described measurement mechanism can record multiple in real timeCounting.
The present invention is finally initial with mensuration according to the girth of described initial count, the second counting, coiler deviceThe time difference of counting and the second counting, obtain the raw materials evaporate amount in the unit interval. Above-mentioned steps of the present inventionSpecifically be preferably the first difference with initial count according to described the second counting, then be multiplied by the girth of coiler device,Obtain the coiling length of axial filament in process that described liquid charging stock becomes steam; Long according to the coiling of axial filament againSpend and hold the cross-sectional area of the utensil of described liquid charging stock, obtain the volume of the liquid that becomes steam; ?Afterwards according to measure initial count and second counting time difference, described in become steam liquid volume withAnd the density of described liquid charging stock, obtain raw materials evaporate amount in the unit interval.
More specifically example can be that metal is changed to liquid state by solid under the state of high-temperature vacuum, works as goldWhen belonging to start vaporizer, ball float is positioned at the A position of metal bath surface, through after a period of time, under ball floatBe down to the B position of liquid level, in this period, corresponding encoder shows that numerical value is C, and axial filament is around axle sleeveThe distance of a upper circle is L, is C*L thereby calculate the distance that ball float declines, then density by metal andThe area of crucible, can calculate raw materials evaporate amount, the i.e. evaporation rate of metal in the unit interval.
Method provided by the invention adopts measurement mechanism to survey the raw materials evaporate amount of chemical vapor deposition stoveFixed, by measuring the displacement of the liquid level decline in liquid evaporation process, obtain the evaporation capacity of raw material. ThisThe measurement assembly that the bright method providing adopts, its buoyant device and coiler device are arranged on the top of raw material,Can reflect in real time the conversion of the liquid level of raw material; Adopt less axial filament and the axle core of thermal coefficient of expansion, andThe testing result that corresponding connected mode obtains is more accurate, can reflect in real time the conversion of raw material, therebyThe accurate ratio of controlling course of reaction Raw, the performance of raising product.
The present invention also provides device or the above-mentioned any one described in a kind of above-mentioned any one technical schemeMethod described in technical scheme is in the application of calculating in solid evaporation capacity. Described solid evaporation capacity is preferably concreteFor, the solid evaporation capacity in one or more situations in closed container, high temperature and vacuum, more preferablyFor the solid evaporation capacity in closed container, high temperature and vacuum. Describedly need to calculate establishing of solid evaporation capacityStandby is chemical vapor deposition stove or single crystal growing furnace, and described measurement mechanism provided by the invention and measuring method are excellentChoosing is specifically applied in chemical vapor deposition stove or single crystal growing furnace.
The invention provides a kind of device and measurement side of the raw materials evaporate amount of measuring chemical vapor deposition stoveMethod, can Real-Time Monitoring and control the evaporation capacity of raw material, has higher accuracy. Especially high temperature,Under the airtight conditions such as vacuum, the present invention adopts axial filament formula to measure, and has reduced the shadow of temperature to parts thermal expansionRing, thereby greatly improved certainty of measurement, and the parts such as metal axial filament and axle core of the present invention's employing,In actual use procedure, security is higher, and connected mode of the present invention, in actual useIn journey, can not affect the requirement of chemical vapor deposition stove to high-air-tightness yet. Experimental result shows, adopts thisThe device of the raw materials evaporate amount of the measurement chemical vapor deposition stove that invention provides, measures chemical vapour deposition (CVD)In journey, the evaporation rate accuracy of raw metal is higher, and deviation is within ± 1.5%.
Referring to Fig. 1, the raw materials evaporate amount of the measurement chemical vapor deposition stove that Fig. 1 provides for the embodiment of the present inventionThe structural representation sketch of device, wherein, 1 is buoyant device, 2 is axial filament, 3 is axle core, 4 is canThe meter showing in real time, 5 is crucible, A and B are that the liquid level in liquid charging stock evaporation process is poor.
In order to further illustrate the present invention, chemical to a kind of measurement provided by the invention below in conjunction with embodimentThe apparatus and method of the raw materials evaporate amount of gaseous phase deposition stove are elaborated, and protection scope of the present invention is notBe subject to the restriction of following examples.
Embodiment 1
First the axle core in measurement mechanism is fixed on to the solid material top in chemical vapor deposition stove, willOne end is connected to axle core and the axial filament that is wrapped on axle core of part hangs down naturally, and by the axle center of axle core withRotary encoder is connected.
Again the other end of axial filament is connected with ball float, and ball float is placed in chemical vapor deposition stoveSolid material top, and make axial filament vertically without varicose.
Fix after above-mentioned measurement mechanism, the solid material heating in crucible is all molten into liquid charging stockAfter, ball float can float over liquid charging stock surface, check and recording measuring device in rotary encoder obtain initially meterNumber, and note keeping axial filament vertically without varicose.
Continue heating, described liquid charging stock is become in the process of steam to the rotary encoder of measurement mechanismRecord the second counting;
Finally according to the girth of described initial count, the second counting, coiler device with measure initial count andThe time difference of the second counting, obtain the raw materials evaporate amount in the unit interval, i.e. the evaporation rate of metal.
Embodiment 2
Utilize chemical vapour deposition technique to produce zinc sulphide, ball float adopts high purity graphite, and axial filament adopts molybdenum filament,The metal filling in crucible is zinc raw material, and when entering after the depositional phase, ball float can be along with under zinc evaporation graduallyFall, thereby embody to the rotating cycle n of coding, and the girth of axle sleeve is L, the time is △ t, holds zinc formerThe area S1 of the crucible of material, the density of zinc is the evaporation rate V that ρ can calculate zinc in the unit interval.Be V=L*n*S1* ρ/△ t, thereby be easy to judge according to the evaporation rate of zinc the intake of hydrogen sulfide. ?780 DEG C of depositing temperatures in zinc sulphide production process, chemical vapor deposition stove internal pressure 10000Pa, raw material is adoptedThe zinc that is 99.999% by purity, utilizes the method, and the conversion ratio of product reaches 73%, zinc evaporation rateHigher with the technological parameter proportion control accuracy of unstrpped gas hydrogen sulfide, deviation is within ± 0.8%.
Embodiment 3
Utilize chemical vapour deposition technique to produce zinc selenide, ball float adopts high purity graphite, and axial filament adopts tungsten filament,The metal filling in crucible is zinc raw material, and when entering after the depositional phase, ball float can be along with under zinc evaporation graduallyFall, thereby embody to the rotating cycle n of coding, and the girth of axle sleeve is L, the time is △ t, holds zinc formerThe area S1 of the crucible of material, the density of zinc is the evaporation rate V that ρ can calculate zinc in the unit interval.Be V=L*n*S1* ρ/△ t, thereby be easy to judge according to the evaporation rate of zinc the intake of hydrogen selenide. ?800 DEG C of depositing temperatures in zinc selenide production process, chemical vapor deposition stove internal pressure 30000Pa, raw material is adoptedThe zinc that is 99.999% by purity, utilizes the method, and the conversion ratio of product reaches 71%, zinc evaporation rateHigher with the technological parameter proportion control accuracy of unstrpped gas hydrogen selenide, deviation is within ± 0.8%.
Above to the device of a kind of raw materials evaporate amount of measuring chemical vapor deposition stove provided by the present invention andMethod is described in detail. Apply a concrete example herein to principle of the present invention and embodimentSet forth, the explanation of above embodiment is just for helping to understand method of the present invention and core think of thereofThink. It should be pointed out that for those skilled in the art, do not departing from the principle of the inventionPrerequisite under, can also carry out some improvement and modification to the present invention, these improvement and modify and also fall into thisIn the protection domain of invention claim.
Claims (10)
1. a device of measuring the raw materials evaporate amount of chemical vapor deposition stove, is characterized in that, comprises,Buoyant device, axial filament, coiler device and the meter composition that can show in real time;
Described buoyant device is placed in the solid material top in chemical vapor deposition stove, described buoyant device withOne end of described axial filament is connected;
The other end of described axial filament is connected with described coiler device, and described coiler device is fixed on chemical gasSolid material top in phase cvd furnace;
The axle center of described coiler device is connected with the described meter that can show in real time.
2. device according to claim 1, is characterized in that, described buoyant device is hollow circuit cylinderBody or hollow sphere.
3. device according to claim 2, is characterized in that, the material of described buoyant device is highPure graphite, C/C composite or quartz; Described axial filament is molybdenum filament, copper wire or tungsten filament.
4. device according to claim 1, is characterized in that, described coiler device is axle core, instituteThe material of stating coiler device is identical with axial filament.
5. device according to claim 1, is characterized in that, described meter is rotary encoder.
6. a method of measuring the raw materials evaporate amount of chemical vapor deposition stove, is characterized in that, comprise withLower step:
A) coiler device in measurement mechanism is fixed on to the solid material top in chemical vapor deposition stove,Buoyant device is placed in the solid material top in chemical vapor deposition stove, and makes axial filament vertically without varicose;
B), while described solid material being all molten into liquid charging stock, described measurement mechanism records initial count;
C) described liquid charging stock is become in the process of steam, described measurement mechanism records the second counting;
D) according to the girth of described initial count, the second counting, coiler device with measure initial count and theThe time difference of two countings, obtain the raw materials evaporate amount in the unit interval.
7. method according to claim 6, is characterized in that, described step D) be specially:
D1) according to described the second counting and the difference of initial count, then be multiplied by the girth of coiler device,Become the coiling length of axial filament in the process of steam to described liquid charging stock;
D2), according to the coiling length of axial filament with hold the cross-sectional area of utensil of described liquid charging stock, obtainBecome the volume of the liquid of steam;
D3) according to the time difference of the initial count of measuring and the second counting, described in become the liquid of steamThe density of volume and described liquid charging stock, obtains raw materials evaporate amount in the unit interval.
8. the side described in device or claim 6～7 any one described in claim 1～5 any oneMethod is in the application of calculating in solid evaporation capacity.
9. application according to claim 8, is characterized in that, described solid evaporation capacity is specially,Solid evaporation capacity in one or more situations in closed container, high temperature and vacuum.
10. application according to claim 8, is characterized in that, the described solid that need to calculate evaporatesThe equipment of amount is chemical vapor deposition stove or single crystal growing furnace.
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