CN1083972C - Pilot oven and application thereof - Google Patents
Pilot oven and application thereof Download PDFInfo
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- CN1083972C CN1083972C CN 96103209 CN96103209A CN1083972C CN 1083972 C CN1083972 C CN 1083972C CN 96103209 CN96103209 CN 96103209 CN 96103209 A CN96103209 A CN 96103209A CN 1083972 C CN1083972 C CN 1083972C
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Abstract
The present invention relates to an experimental furnace used for processing the sample under the temperature gradient. The experimental furnace can be used for preparing the high temperature superconducting yttrium, barium, copper, and oxygen component in the melt-textured method. The purposes of the present invention is to find out the resolution method, one or more than one samples are processed under the similar temperature gradient as far as possible, but each sample has different temperature condition each other. The resolution method of the present invention is that at least one heat insulation wall 1 is introduced and divided into at least two subareas 4a and 4b, the uniform distribution is in each area, the temperature is different and mutually independent, at least one sample area 5c in the heat insulation wall 1 is used for placing the sample processed by the temperature.
Description
The present invention relates to an experimental furnace and in the application that is equipped with high-temperature superconductor yttrium barium copper oxide (YBCO) body material with the melting texture legal system.This experimental furnace also can be used in the preparation of other materials that need use thermograde.
In general, Guan Hanglu or block furnace can be made up of the single or multiple thermals treatment zone.These stoves can produce a certain size but the maximum thermograde that is about 25K/cm for diameter more than or equal to the sample of 30mm, and generally are difficult to accomplish the treatment of different temperature simultaneously a plurality of samples set arbitrarily in same stove.In addition, in existing Bridgeman method, sample can be in stove along the thermograde direction (German patent DE-OS3223064), but this design also only allows a plurality of samples are carried out same Temperature Treatment of moving.
In the investigation of materials field, people wish just can carry out Temperature Treatment same or that the specified temp difference is arranged to a plurality of samples in same experiment just.
It is a kind of common Temperature Treatment process that the melting texture legal system is equipped with high-temperature superconductor yttrium barium copper oxide (YBCO) body material, sample by the initial powder material of various compositions (as YBa
2Cu
3O
x, Y
2BaCuO
5, Y
3O
2, PtO
2, Ag
2O etc.) compacting forms.One of purpose of this Temperature Treatment is to improve the performance such as the critical current density of sample for different application.Temperature Treatment process commonly used is so-called MTG-Process or modiried is MTG-Process [S.Jin, T.H.Tiefe1, R.C.Sherwood, R.B.van Dover, G.W.Kammlot, R.A.Fastnacht, Phys.Rev.B37 (1988) 7850].In this process, sample at first is heated to more than the peritectic reaction temperature, and the short time stop, then through or without a quenching process to a certain temperature.After this sample is through a slow cooling procedure and carry out the peritectic reaction process and form YBa
2Cu
3O
xCrystal.Slow cooling procedure begin and during, sample is in 0 ℃/cm to 200 ℃/cm thermograde, along with temperature reduces, the peritectic reaction temperature Tp is also gone to the other end of heat lentamente from a colder end of sample, that is to say YBa
2Cu
3O
xCrystal is long continuously to the other end from an end of sample.Though can directly read the peritectic reaction temperature Tp from phasor under the thermodynamical equilibrium situation in principle, the process in the reality all is a dynamic process, need a supercooling temperature.Actual peritectic reaction temperature is Tr=Tp-T.The peritectic reaction temperature Tp depends mainly on the concrete composition of sample.And the size of supercooling temperature T also is decided by the preliminary treatment before peritectic reaction except that the concrete composition that is decided by sample.Because the sample treatment process reaches a week, finding out optimum process condition just becomes very time-consuming process.
Therefore, the objective of the invention is to design an experimental furnace, handle so that can be simultaneously one and more than one sample be carried out same design temperature process, and temperature conditions that again might be in addition different to different samples.Purpose of the present invention in addition also is to find out the optimal parameter that melting texture prepares high-temperature superconductor yttrium barium copper oxide (YBCO) body material sample, particularly significantly reduces the time of finding out best initial temperature, and with thus obtained parameter as the master data of producing in batches.
The purpose of the invention described above has obtained solution in all kinds of patents claim.
Precondition of the present invention is to have to have more than two the stove of the thermal treatment zone of temperature control separately at least, such as one six equal block furnaces of temperature control heating separately.The control of each heating surface can be controlled by power or temperature and realize.
In such stove, add one side position at least and direction is all transformable, thermal conductivity is relatively poor insulated wall, can have even distribution in the subregion that is separated by this wall but be equipped with temperature inequality.The insulated wall shape of using among the present invention and size should be with burner hearth corresponding so that can not carry out the exchange of cross-ventilation and hot irradiation between each subregion that is spaced.Under above-mentioned prerequisite, use more than one insulated wall also to belong within the present invention.
At least should have a sample area to can be used for placing to need the sample of handling in insulated wall of the present invention, each sample area can be placed at least one sample in separated from each other and each sample area in insulated wall.
The used insulated wall of the present invention should be used relatively poor material of thermal conductance such as Al
2O
3Pottery.The width of insulated wall, the kind of material, the shape of sample area and distribution all should change according to different requirements.Concrete insulated wall width is mainly determined by the size of thermograde between the required different subregions and sample.
The present invention also is not limited to be parallel to the insulated wall of horizontal plane, perhaps is limited to the use block furnace, only need consider the coincideing of inwall of insulated wall and burner hearth when using the stove of other types, is that then situation is simple especially for example with the block furnace.
Following the present invention describes in detail for example with schematic diagram.
Fig. 1 is the sectional view of block furnace, comprising the cross section of possible one side insulated wall of the present invention and relative other structures of stove thereof, and obtainable thus Temperature Distribution.
Fig. 2 is along the cross section of the A-A line of Fig. 1 and corresponding Temperature Distribution.
Fig. 3 is the possible insulated wall design of another kind of the present invention.
Fig. 4 a is equipped with the temperature course schematic diagram of high-temperature superconductor yttrium barium copper oxide (YBCO) body material sample for existing MTG legal system.
Fig. 4 b is equipped with the temperature course schematic diagram of high-temperature superconductor yttrium barium copper oxide (YBCO) body material sample for existing Modified MTG legal system.
Fig. 5 prepares the position distribution of yttrium barium copper oxide (YBCO) body material sample and sample area thereof for a kind of possible melting texture.
Fig. 6 prepares the position distribution of yttrium barium copper oxide (YBCO) body material sample and sample area thereof for another kind of possible melting texture.
Fig. 1 has schematically illustrated the four sides stove inwall 3 of the block furnace of band heater 2.Burner hearth in the furnace wall has one side insulated wall 1, this wall 1 is divided into two subregion 4a and 4b to burner hearth, because this two subregion each has the heater 2 of temperature control separately, so respectively there is one evenly to distribute in this two subregion within it, but the temperature (T1: T2) that can have nothing in common with each other, in insulated wall 1, produce thermograde Δ T=(T1-T2)/L like this, shown in the last figure of Fig. 1.Insulated wall 1 in this example can be used aluminium oxide ceramics, and arranges sample area 5 compositions separately to be used to place sample 6 by three.
For example, supposing that the temperature at subregion 4a is 1360 ° of K, be 1170 ° of K in the temperature of subregion 4b, and the thickness of insulated wall is L=60mm, and producing one so at sample 6 places is linear 30 ° of K/cm of thermograde basically.Provide different insulated wall thickness and provide different 4a and the subregional temperature difference of 4b, just can be created in different thermograde in the 0-300 ° of K/cm scope.It is emphasized that in thermograde to be that the situation of 0 ° of K/cm uses insulated wall of the present invention also can bring some advantages on some is used.
The inside dimension of burner hearth in this example (Fig. 1) is under the situation of 20 * 20cm, and the size shape of insulated wall 1 need be fit to the inwall of burner hearth, and to be divided into three parts for well.For example insulated wall 1 can be made up of the honeycomb wall frame 1b that contains a plurality of sample areas 5, and the both sides of wall frame 1b communicate (placing sample easily), and both sides are added two plane wallboard 1a and are closed and get final product.
Illustrated the cross section situation of Fig. 1 among Fig. 2 along the A-A line.
It is that example is illustrated that application of the present invention will be equipped with high-temperature superconductor yttrium barium copper oxide (YBCO) body material with the melting texture legal system below.The diameter of the sample of handling as need 6 is 35mm, and the size of sample area 5 can be 40 * 40 * 40mm so, the desirable 10mm of wall 1a thickness, and subregion district 4a, the temperature difference of 4b can be 90 ° of K.Though the present invention is not only limited to three separation structures (1a-1b-1a) of insulated wall, this structure is owing to different materials (thermal conductivity) and the thickness thereof of replacing each several part easily, so can the very wide condition of different temperatures of reach in practical operation.
Fig. 3 has illustrated the another kind of compound mode of insulated wall among the present invention, under the corresponding prerequisite of size dimension that as far as possible keeps sample area and sample, that is to say that keeping sample can change the possibility and the advantage thereof of its position under the situation of needs again in the space around as far as possible reducing sample.Insulated wall of the present invention is made up of several little minute wall 7 in this kind compound mode, and Fig. 3 has only schematically drawn nearer one, and each little minute wall 7 should contain the sample area 5 of at least one openings at one side.Each sample area of Fig. 3 illustrated can have different sizes, and can stagger mutually again in the position in minute wall.Sample just can be put into minute wall one by one burner hearth inside and form the insulated wall 1 described in the invention after sample area is put well.
Within the scope of the invention, also comprised following content, promptly by using the heater 2 of homogeneous heating, closing on the inboard wall of burner hearth of this heater, and in the subregion, produced the even temperature distribution, putting the remaining space that should reduce as best one can between inboard wall of burner hearth and the insulated wall 1 before this.
What is called among the present invention " sample " has more than and is limited to the simple solid that does not have shell, sample such as also can be placed in the crucible, and what place in the sample area like this is exactly crucible and sample wherein.
The even temperature of indication distributes among the present invention, be not restricted to evenly distribute according to the accurate of definition, as constant and known non-homogeneous Temperature Distribution also at the row of indication.
Same application also can be used for the designed industrial furnace according to the present invention.
Here underline once more, the dimensional orientation of insulated wall 1 in stove can change arbitrarily.Such as then better when the grown crystal with the orientation of horizontal direction.
Content of the present invention also comprises following scope, i.e. the position changeable of sample 6 in each sample area 5, or the position of sample area itself is also variable.Make each sample when accepting Temperature Treatment, can have different temperature courses like this.The possibility that these the present invention comprised has special significance in investigation of materials.And these possibilities will be below the special case of an application by experimental furnace of the present invention explain detailedly.
Fig. 4 a and 4b illustrate the situation of the temperature course of melting structure high-temperature superconductor yttrium barium copper oxide (YBCO) body material generally speaking.
Fig. 5 and 6 has schematically illustrated four heaters 2 of a square burner hearth inwall 3.Burner hearth is inner by patent ... (patent application 19506503.4) adds one side insulated wall 1, stove is divided into two parts subregion 4a and 4b thus, every part all has an even temperature to distribute, but temperature can (T1: T2) inequality separately, in insulated wall, produce a thermograde Δ T=(T1-T2)/L thus, shown in figure on Fig. 5 and 6.Insulated wall 1 can be by being formed as aluminium oxide ceramics, is divided into from top to bottom four row's sample areas placing sample in these row, also several sample areas can be arranged in the direction of vertical paper.By change T1, T2, the direction of L and insulated wall 1, thermograde can and change on the direction in space in 0-300 ° of K/cm magnitude range arbitrarily.Provide in the insulated wall 1 after a certain size the thermograde Δ T, the temperature of sample just can change by changing its position at every turn, that is to say, the sample in insulated wall 1 by its position-adjustable to having identical or random different temperatures.
As Tax is temperature when adding that the slow cooling at lowest temperature place of the sample behind the thermograde Δ T is initial, considering that the crystal nucleation process simultaneously, the best initial temperature Tao that a certain prior the unknown is arranged concerning the sample with certain actual peritectoid reaction temperature Tr, this temperature should be on actual peritectoid reaction temperature Tr the several years, it is too of a specified duration that high again initial temperature can make sample stop under too high state of temperature meaninglessly, thereby cause that effect that some is unnecessary such as too much liquid phase run off.Too low on the other hand initial temperature also can produce many spontaneous nucleation, causes growing up to rather than desirablely growing up to single megacryst of a lot of small crystals.
Supposing that the temperature at subregion 4a is 1360 ° of K, be 1170 ° of K in the temperature of subregion 4b, and the thickness of insulated wall is L=60mm, and producing one so at sample 6 places is linear 30 ° of K/cm of thermograde basically.Provide different insulated wall thickness and provide different 4a and the subregional temperature difference of 4b, just can be created in different thermograde in the 0-300 ° of K/cm scope.
According to the present invention, the several samples 6 with same real reaction temperature T r are placed to different position in the insulated wall 1.This can realize by the mode of Fig. 5, and promptly each sample area 5 is at the location dislocation of insulated wall 1, and simultaneously each sample 6 at the invariant position of the sample area 5 at place.But also can realize by the mode of Fig. 6, i.e. the invariant position of each sample area 5 in insulated wall 1, and simultaneously each sample 6 at the location dislocation of the sample area 5 at place.Each sample is all through a slow temperature-fall period of the MTG that knows in given thermograde Δ T, and the initial temperature Tax of each sample is slightly different each other, as illustrated in Figures 5 and 6.When enough sample numbers are arranged, as can once handling under the situation that reaches 20 samples in the circulation without a doubt in practice, the possibility of the best initial temperature Tao of one of them sample 6 experience is just very big, and test as standard the melting texture of sample after this resulting thus sample and sample area position, to obtain to have the sample of desirable high critical current densities and bulky crystal.Thermograde is 30 ° of K/cm in this example, and the variation of sample position 1mm is corresponding to the variations in temperature of 3 ° of K.
The possibility of another kind of operation is, under the situation of initial temperature Ta, finds out the sample that has best real reaction temperature T r accordingly given, and its method is that the sample 6 with different real reaction temperature T r is positioned on the same position in the insulated wall 1.Also can find the sample composition deviation that meeting occurs in the manufacturing process in this way soon.
As a same reason, the Temperature Distribution that occurs at heating subregion 4a and 4b inhomogeneous also can obtain by the minor alteration of each sample position revising, thereby can obtain well sample of repeatability when reaching a large amount of production.
Number symbol table 1-insulated wall 1a-wallboard 1b-wall frame 2-heater 3-stove inwall 4a, heating subregion 5-sample area, the 6-sample 7 of 4b-different temperatures-minute wall Tax-when sample lowest temperature place slow cooling is initial
The thickness of temperature L-insulated wall 1
Claims (9)
1, an experimental furnace, form by burner hearth and wherein heater (2) and stove inwall (3), its burner hearth is divided into two subregions that can have different temperatures at least, it is characterized in that: the insulated wall (1) of one side poor thermal conductivity is positioned in the burner hearth and burner hearth and is divided at least two subregion (4a that can have mutual incoherent different temperatures at least, 4b), each subregion interior temperature distribution is even, and the shape size of insulated wall (1) is corresponding to inboard wall of burner hearth and should be as far as possible have a sample area (5) at least in order to place by the sample of Temperature Treatment near in thirty years of age and the insulated wall (1).
2, experimental furnace according to claim 1 is characterized in that: a plurality of sample areas (5) are arranged in the insulated wall (1).
3, experimental furnace according to claim 1 and 2 is characterized in that: insulated wall (1) is made up of the wall unit that can piece together or combine (1a, 1b, 7).
4, experimental furnace according to claim 3 is characterized in that: insulated wall (1) is made up of the wall frame (1b) that has comprised sample area (5) between the plane wallboard (1a) of two variable thickness and two plates.
5, experimental furnace according to claim 4 is characterized in that: wall frame (1b) is frame type structure, and contained a plurality of sample areas (5) distribute as the cellular rule that is.
6, experimental furnace according to claim 4 is characterized in that: insulated wall (1) is made up of the branch wall (7) of a plurality of independent shapings.
7, according to the application of the described experimental furnace of one of aforementioned each claim, it is characterized in that: high-temperature superconductor yttrium barium copper oxide (YBCO) body material sample (6) is positioned in the sample area (5) as follows:
-sample (6) with different real reaction temperature (Tr) is placed on the same position of insulated wall (1), perhaps
-sample (6) with identical real reaction temperature (Tr) is placed on the diverse location of insulated wall (1),
Each sample under given thermograde Δ T separately through a slow temperature-fall period.
8, the application of experimental furnace according to claim 7 is characterized in that: the change of sample (6) position realizes that in the change of the position of insulated wall (1) position of each sample (6) in sample area (5) but remains unchanged by sample area (5).
9, the application of experimental furnace according to claim 7 is characterized in that: the change of sample (6) position realizes that by the change of the position of each sample (6) in sample area (5) each sample area (5) but remains unchanged in the position of insulated wall (1).
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19506503.4 | 1995-02-24 | ||
| DE1995106503 DE19506503C1 (en) | 1995-02-24 | 1995-02-24 | Laboratory furnace esp. for research into materials |
| DE19603362.4 | 1996-01-23 | ||
| DE1996103362 DE19603362A1 (en) | 1995-02-24 | 1996-01-23 | Use of a laboratory oven |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1135037A CN1135037A (en) | 1996-11-06 |
| CN1083972C true CN1083972C (en) | 2002-05-01 |
Family
ID=26012780
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96103209 Expired - Fee Related CN1083972C (en) | 1995-02-24 | 1996-02-26 | Pilot oven and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1083972C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB201112610D0 (en) * | 2011-07-22 | 2011-09-07 | Rec Wafer Norway As | Heating a furnace for the growth of semiconductor material |
| CN102519253B (en) * | 2011-10-27 | 2014-02-26 | 中钢集团洛阳耐火材料研究院有限公司 | Fireproof material slag resistance experiment method and furnace |
| CN107699673B (en) * | 2017-10-12 | 2019-05-31 | 钢铁研究总院 | A kind of high throughput gradient thermal processing array crucible |
| CN110857842A (en) * | 2018-08-22 | 2020-03-03 | 中国航发商用航空发动机有限责任公司 | Heat treatment furnace and oxidation test method |
-
1996
- 1996-02-26 CN CN 96103209 patent/CN1083972C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1135037A (en) | 1996-11-06 |
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