CN1162045C - Heater with MoSi2 base and method of manufacture thereof - Google Patents
Heater with MoSi2 base and method of manufacture thereof Download PDFInfo
- Publication number
- CN1162045C CN1162045C CNB008001928A CN00800192A CN1162045C CN 1162045 C CN1162045 C CN 1162045C CN B008001928 A CNB008001928 A CN B008001928A CN 00800192 A CN00800192 A CN 00800192A CN 1162045 C CN1162045 C CN 1162045C
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- China
- Prior art keywords
- density
- heater
- sintering
- central part
- presintering
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/148—Silicon, e.g. silicon carbide, magnesium silicide, heating transistors or diodes
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/018—Heaters using heating elements comprising mosi2
Abstract
There is provided an MoSi2-based heating element having improved durability, and a method for inhibiting the formation of defects during the processes for manufacturing such an MoSi2-based heating element. The MoSi2-based heating element is a heating element containing 70% or more MoSi2 in which the difference between the average density of the entire heating element and the density of the central portion corresponding to one fifth of the diameter of the heating element (true density ratio) is 5% or less, preferably 3% or less. In the process of temporary sintering, sintering is performed in a temperature pattern of an adequately adjusted temperature raising rate.
Description
Technical field
The present invention relates to contain 70% above MoSi
2The heater of (molybdenum silicide) (comprises that the whole compositions that constitute heater and material thereof are MoSi
2Object.Described in this manual " heater " and " heating material " all use by this implication.) and manufacture method, particularly relate to the whole averag density of a kind of heating material (base material) and the central part that is equivalent to heater diameter 1/5 (hereinafter, except specifying, all " central parts " all refers to be equivalent to the core of heater diameter 1/5.) the heater and the manufacture method thereof of the little and whole sintering equably of base material of density contrast (real density than).
Background technology
With MoSi
2In the manufacturing process for the heater of principal component, at first the raw material (MoSi of adjusted to predetermined particle diameter
2) powder mixes with the shaping assistant of water, organic bond etc. with clay mineral (bentonite etc.), by extrusion molding it is shaped to predetermined shape then, and is for example bar-shaped.
By drying or degreasing process those water that no longer need after moulding or organic bond etc. are removed from formed body then.At this moment the real density of formed body ratio is generally 50～70%.In order to prevent this formed body oxidation, generally in neutrality or reducing atmosphere, carry out presintering (being also referred to as once sintered), at this moment the real density of this formed body ratio rises to 70～95%.
Then the presintering body of such acquisition is placed oxidizing atmosphere (comprising atmosphere), feed electric current to this presintering body itself, thereby it is carried out resistance heating (energising sintering).By this energising sintering, generally can on the surface of sintered body, form oxide-film, make its real density ratio be increased to 90～100% simultaneously, thereby finally made the parts that are used to constitute heater.At last, generally weld together by heat generating part and the portion of terminal that same material constitutes, so far just can provide use by electric weld handle.
In the prior art, for being generally bar-shaped exothermic material, relation between its inside and outside two-part density contrast and the exothermic material performance is not fully found out as yet, in addition, in the operation that above-mentioned presintering and energising sintering are carried out continuously, be used to make the method for sintered density homogenizing yet not find out.Present inventors have obtained following discovery by the result of further investigation.
General for bar-shaped calandria, if the not enough 9mm of its diameter, then its influence (density contrast) is less, but for the major diameter exothermic material more than the 9mm, can not carry out uniform sintering, in a single day and its density contrast begins to increase gradually, and reaches more than the 15mm, it is very obvious that following problem just becomes.Though have the diameter of some heaters slightly to reach 24mm, diameter is thick more, the trend that density contrast increases is obvious more.
Just produce the base material of density contrast for those when the presintering, even by electric sintering circuit it is carried out sintering again, can not dwindle its density contrast, therefore, still residual lower density is poor in the final products that become heater.
The exothermic material that there is density contrast in those at the central part and the periphery of presintering body (once sintered body), heart portion produces the porous part of a kind of being called " pore " therein when the energising sintering, will produce stress owing to the difference that exothermic material itself expands like this, thereby cause the generation of crackle.In addition, under the situation of welding same diameter base material,, therefore also there is the problem that cracks etc. at weld part because the hardness of central part and periphery there are differences.In addition, the low temperature resistant oxidation susceptibility of low density core is good inadequately, in case therefore oxidized easily and therefore powdered gradually when aerobic is sneaked into, this just becomes one of disrumpent feelings easily in use reason in the clamping position of heater.
Summary of the invention
The present invention will overcome above-mentioned shortcoming, provides a kind of with MoSi
2For principal component and in the heater and the manufacture method thereof of the minimum excellent heat resistance of the density contrast of the central part of heater and periphery, by heating material being carried out presintering and the energising sintering is being made in a series of manufacturing processes of heater, can alleviate the problem of the porous part that is called as " pore " that produces at central part and because the stress that the difference of exothermic material expansion causes causes the problem of crackle.In addition, the present invention can be used for suppressing the generation of heater be full of cracks when welding and preventing because the breakage of the caused heater of low-temperature oxidation of central part.
Present inventors have carried out deep research in order to solve above-mentioned problem, found that, by resembling the density of controlling exothermic material following, the useful life that can improve heater.In addition, present inventors have also found a kind of control method.
1. one kind with MoSi
2Be the heater of principal component, wherein contain the MoSi more than 70%
2, it is characterized in that poor (real density than) of the averag density of heater integral body and the density of the central part that is equivalent to heater diameter 1/5 is below 5%.
2. above-mentioned 1 is described with MoSi
2Heater for principal component is characterized in that, poor (the real density ratio) of the above-mentioned density of the averag density of heater integral body and central part is below 3%.
3. one kind with MoSi
2Manufacture method for the heater of principal component is characterized in that, poor (real density than) of the density of the ensemble average density of heater and the central part that is equivalent to this heater diameter 1/5 below 5%, is characterized in that, makes and contains 70% above MoSi
2Exothermic material in 5～15 hours, slowly be warmed up at least 1350 ℃ to 1650 ℃ scope, under this temperature, carry out presintering, till poor (real density than) of the density of the ensemble average density of heating material and the central part that is equivalent to this heating material diameter 1/5 becomes below 5%, then to its sintering of switching on.
4. above-mentioned 3 is described with MoSi
2Manufacture method for the heater of principal component is characterized in that, poor (real density compares) of the ensemble average density of the heater behind heating material after the presintering and the energising sintering and the above-mentioned density of central part is below 3%.
Simple declaration to accompanying drawing
Fig. 1 is the curve chart of the heat temperature raising model of expression comparative example and embodiment.
Fig. 2 is the key diagram that expression produces defective (pore) when the low presintering body of sintered density switched on sintering.
Fig. 3 is the key diagram that expression produces defective (crackle) when the high presintering body of sintered density switched on sintering.
To be expression produce the key diagram of defective (crackle) to two bar-shaped sintered bodies switch on when welding to Fig. 4.
Fig. 5 is illustrated in the key diagram that the sintering heater is carried out low temperature resistance to oxidation when test heating-up temperature circulation (200 ℃～480 ℃).
Embodiment of the present invention
With MoSi
2For the heating material of principal component can carry out presintering (once sintered) being heated under 1400～1650 ℃ the condition, but in this presintering operation, the central part and the periphery of presintering body have produced density contrast, and this is because the periphery that heating material conducts heat easily will begin the cause of sintering prior to central part.
In the presintering operation, have only periphery to begin sintering earlier, make therefore to have produced arch formation by the solid bed that on the section of presintering body, forms ring-type, thereby cause shrinking the difficulty that becomes towards the sintering of central part.It is high that the result makes that the density of base material central part does not resemble the density of periphery, thereby produced density contrast.
As mentioned above, in case in presintering, produced the sintered body of density contrast,, the density contrast of this presintering body is dwindled even come acceleration of sintering by the different energising sintering (resistance heating) of mode of heating.
In order to address this problem, when presintering, should carry out sintering according to the mode that can not produce arch formation.
Usually during the sintering at conducting powder end, generally form the order that (shrinking less) → neck growth (shrinking bigger) → pore spreads to the outside and be accompanied by contraction and carry out densification according to neck.
Yet as large diameter sintered body, owing to the influence of conducting heat produces temperature difference, the result changes contraction speed at its periphery (near surface) and central part.
For example, big when the central part of presintering begins to form neck, carried out the growth of neck at periphery.Therefore, according to the presintering that simple temperature model (constant speed intensification, constant temperature maintenance etc.) in the past carries out, particularly this tendency is more strong in the major diameter sintered body, is easy to generate arch formation.
In order to suppress this phenomenon, should supply with MIN necessary energy at any time according to the progress of sintering, so that make it that undesirable substance transfer (only producing significant contraction etc. at periphery) not take place.That is to say, to containing 70% above MoSi
2Heating material in the short time after heat temperature raising to 1000～1300 ℃, spend 5～15 hours again it is warmed up at leisure from least 1350 ℃ to 1650 ℃ scope, carry out presintering with this understanding, so that be reduced to below 5% at the central part of heating material section part and the density contrast of periphery (real density ratio).
Can think that above result is owing to the sintering velocity unanimity in base material integral body, thereby make the cause of carrying out equably towards the sintering contraction of center position.
Like this, present inventors when carrying out presintering, sintering under the temperature model of adjusting programming rate aptly, therefore, even under the situation of large diameter presintering body, also can obtain a kind of at the central part of this presintering body and the very little sintered body of density contrast of periphery.
That is to say, can obtain a kind of central part of presintering body section and the density contrast of periphery (real density ratio), even can obtain a kind of this density contrast (real density ratio) at the presintering body below 3% at the presintering body below 5%.
Should illustrate, said central part resembles and is meant the core that is equivalent to heater diameter 1/5 above-mentioned, in order to measure the density of this central part, central part can be fixed and periphery be chipped away till its diameter becomes 1/5 (becoming 1.8mm from original diameter 9mm) of its original diameter, with at this moment averag density density (real density) as this central part with lathe.In addition, the mensuration of density Archimedes's method is routinely carried out.
The presintering body that so the obtains sintering of about 1700 ℃, switching on, the global density of sintered body is improved equably, and become the good heater of a kind of durability.
So the heater that obtains can not produce pore or be full of cracks in manufacturing process, even and when heater welding that will be bar-shaped, can not produce the crackle that the density contrast owing to central part and periphery causes yet.In addition, this heater in use can be owing to its inside (particularly producing under the situation of pore) optionally oxidation and carry out efflorescence and cause from the problem of heater content broken yet.
Embodiment and comparative example
With a kind of 70% above MoSi that contains
2Heating material be shaped and degreasing, obtain the bar-shaped formed body of a kind of 11mm, this formed body is carried out presintering according to the heat temperature raising model shown in a～d of Fig. 1.
A～b of Fig. 1 represents comparative example 1 and 2, and c～d of Fig. 1 represents embodiments of the invention 1 and 2.Averag density when various heat temperature raising models according to a～d being shown in the table 1 carrying out presintering and the density of central part and averag density and central part density poor.Should illustrate that a～d of Fig. 1 is corresponding with a～d of table 1.
For according to simple heat temperature raising model just the heat temperature raising model a～b of table 1 carry out the comparative example 1 and 2 of sintering, produce 5.7%～10.3% density contrast between the ensemble average density of presintering body and the density of central part.
In contrast, for the embodiment of the invention 1 and 2 of supplying with the necessary energy of bottom line according to the progress of sintering at any time, just carry out the situation of sintering, can obtain a kind of density contrast and have only 0.3%～2.8% so little presintering body according to heat temperature raising model c～d.
Table 1
| Temperature model | (a) | (b) | (c) | (d) |
| The averag density of base material integral body (%) | 86.0 | 93.5 | 91.2 | 91.5 |
| The density of central part (%) | 75.7 | 87.8 | 88.4 | 91.2 |
| Poor (%) of averag density and center density | 10.3 | 5.7 | 2.8 | 0.3 |
Density is represented with real density.
Investigation produces the situation of defective when the low presintering body of sintered density is switched on sintering below.
The real density of using whole sintering equably than be 88% presintering body (embodiment 3) and central part and periphery have a density contrast carry out the presintering body of the comparative example 1 of sintering according to heat temperature raising model a, under 1700 ℃, carry out 2 minutes energising sintering.
Even the embodiment 3 that carries out even sintering when presintering also sintering equably when the energising sintering, its real density has reached 99%.On the other hand, exist density contrast comparative example 1 the presintering body energising during sintering the material of low density central part attracted to periphery, produced pore at central part as shown in Figure 2.
The section of the bar-shaped body periphery of symbol 2 expression presintering, the section of symbol 3 expression central parts.In addition, as can be seen from Table 1, the average presintering density among Fig. 2 is 86.0%, and the density of central part 3 is 75.7%.
Test 2
Investigation produces the situation of defective when the high presintering body of sintered density is switched on sintering below.
The real density of using whole sintering equably than be 92% presintering body (embodiment 4) and central part and periphery have a density contrast carry out the presintering body of the comparative example 2 of sintering according to heat temperature raising model b, under 1700 ℃, carry out 2 minutes energising sintering.
The embodiment 4 that carries out even sintering when presintering is still intact behind the energising sintering, but the presintering body of comparative example 2 that has a density contrast when the energising sintering because central part cracks 4 with different the elephant as shown in Figure 3 of the thermal expansion of periphery when lowering the temperature.The section of the periphery of the bar-shaped body of symbol 5 expression presintering, the section of symbol 6 expression central parts.
In addition, as can be seen from Table 1, the average presintering density in Fig. 3 is 93.5%, and the density of central part 6 is 87.8%.
Test 3
Investigation produces the situation of defective when the energising welding below.
2 presintering bodies of the embodiment 1 that density contrast shown in the C of his-and-hers watches 1 is less (average presintering density 91.2%, the density 88.4% of central part, density contrast 2.8%) sintering of switching on.The result of energising sintering does not produce above-mentioned " pore " or crackle.
As shown in Figure 4, make the heater of elongate objects in order to use 2 rods 8,9, with end face 10 contacts of the two, on one side energising, pressurization is with the welding of switching on one side.
When welding energising solder side deform owing to being extruded, and at this moment, the bar-shaped presintering body that has a density contrast is owing to the nonhomogeneous hardness of central part and periphery produces the crackle 7 that resembles as shown in Figure 4.
On the other hand, under the situation that the sintered body (suitable at the embodiment below 0.3% 2 with density contrast) after using the very little energising sintering of density contrast welds, on solder side, do not crack fully during welding.
Because as can be seen, under the situation that obviously distortion takes place, therefore wish that its density contrast is little of 2.0% to 2.8% still not ideal enough even the density contrast of periphery and central part is little, preferably little to below 1%.
Test 4
The real density of using whole evenly sintering than be the energising agglomerated material (embodiment 5) of 95.0% 18mm and the sintered density of on average switching on be 95.2% and central part density be 83.0% energising agglomerated material (comparative example 3), carry out the low temperature resistance to oxidation and test.
Various base materials are cut into the length of 100mm, make it in atmosphere, stand temperature cycles shown in Figure 5 (200 ℃～480 ℃) repeatedly.In this temperature province, can not form the good SiO of oxidative resistance
2Overlay film, so Mo and Si are oxidized simultaneously and become powdery.
After through 100 circulations two kinds of base materials are compared, for the base material that has density contrast (comparative example 3), the density of its central part is low, therefore big with the contact area of oxygen, so oxidation is carried out soon,, do not maintain original shape from the efflorescence gradually of its inside.
On the other hand, for the high density base material that does not have density contrast, though in its skin section a spot of efflorescence is arranged, portion does not have oxidation fully within it, remains intact.
Therefore as can be seen, when it was switched on as heater, the base material that the density at central part and periphery in the past there are differences was by breakage, and still goods of the present invention are not then by breakage, and its durability is good.
Industrial applicibility
The temperature model of adjusting aptly programming rate according to the present invention carries out presintering, can make the sintering velocity of base material integral body consistent, thereby so that carry out equably towards the sintering shrinkage of center position, even in the situation of major diameter presintering body, also can obtain the very little sintered body of the density contrast of a kind of central part and periphery. That is to say, can obtain a kind of on the presintering body section central part density and poor (the real density ratio) of averag density below 5%, even at the presintering body below 3%.
By this presintering body is carried out final sintering at about 1700 ℃ of lower resistance sinterings, the global density of this sintered body rises equably when resistance sintering, therefore can obtain the good heater goods of durability.
The heater goods that so obtain can not produce pore or be full of cracks in a series of manufacturing process, even and can not crack owing to the density contrast of central part and periphery when bar-shaped heater is welded yet. In addition, the advantage of this heater is in use can be owing to the problem that selective oxidation and efflorescence cause the heater content broken occurs its inside (particularly producing in the situation of pore).
Claims (2)
1. one kind with MoSi
2Manufacture method for the heater of principal component is characterized in that, the ensemble average density of this heater and the real density of the density of the central part that is equivalent to this heater diameter 1/5 than 5% or below, the step that this method comprises is:
Make and contain the above MoSi of 70 weight %
2Exothermic material, after temperature is raised to 1000-1300 ℃, in 5～15 hours, slowly be warmed up at least 1350 ℃ to 1650 ℃ scope,
Described heater is carried out presintering, till the real density ratio of the ensemble average density of heating material and the density of the central part that is equivalent to this heating material diameter 1/5 becomes below 5%, then
To its sintering of switching on.
2. claim 1 is described with MoSi
2Manufacture method for the heater of principal component is characterized in that, this heating material behind the energising sintering, the ensemble average density of heater and the real density of the above-mentioned density of central part than 3% or below.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP42780/1999 | 1999-02-22 | ||
| JP11042780A JP3070742B1 (en) | 1999-02-22 | 1999-02-22 | Heating element mainly composed of MoSi2 and method of manufacturing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1294833A CN1294833A (en) | 2001-05-09 |
| CN1162045C true CN1162045C (en) | 2004-08-11 |
Family
ID=12645496
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB008001928A Expired - Lifetime CN1162045C (en) | 1999-02-22 | 2000-02-17 | Heater with MoSi2 base and method of manufacture thereof |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP1026920B1 (en) |
| JP (1) | JP3070742B1 (en) |
| CN (1) | CN1162045C (en) |
| WO (1) | WO2000051399A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9534398B2 (en) | 2013-03-13 | 2017-01-03 | Columbia Insurance Company | Patterned tiles and floor coverings comprising same |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004214075A (en) * | 2003-01-07 | 2004-07-29 | Nikko Materials Co Ltd | HEATING ELEMENT CONTAINING MoSi2 AS MAIN CONSTITUENT |
| JP4823486B2 (en) * | 2004-03-29 | 2011-11-24 | Ｊｘ日鉱日石金属株式会社 | Heater mainly composed of MoSi2 having excellent pest resistance and method for producing the same |
| WO2023161197A1 (en) | 2022-02-23 | 2023-08-31 | Universita' Degli Studi Di Roma "La Sapienza" | Method for the characterization of short peptides from industrial hemp |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE7513997L (en) * | 1975-12-11 | 1977-06-12 | Bulten Kanthal Ab | PROCEDURE FOR THE MANUFACTURE OF SILICOR CARBID MOLDINGS |
| JPH03141162A (en) * | 1989-10-26 | 1991-06-17 | Riken Corp | Production of molybdenum disilicide heater |
| WO1998011568A1 (en) * | 1996-09-13 | 1998-03-19 | Tdk Corporation | Ptc thermistor material |
-
1999
- 1999-02-22 JP JP11042780A patent/JP3070742B1/en not_active Expired - Fee Related
-
2000
- 2000-02-01 EP EP20000300768 patent/EP1026920B1/en not_active Expired - Lifetime
- 2000-02-17 WO PCT/JP2000/000895 patent/WO2000051399A1/en active Application Filing
- 2000-02-17 CN CNB008001928A patent/CN1162045C/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9534398B2 (en) | 2013-03-13 | 2017-01-03 | Columbia Insurance Company | Patterned tiles and floor coverings comprising same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3070742B1 (en) | 2000-07-31 |
| EP1026920B1 (en) | 2007-08-22 |
| CN1294833A (en) | 2001-05-09 |
| JP2000243538A (en) | 2000-09-08 |
| EP1026920A2 (en) | 2000-08-09 |
| EP1026920A3 (en) | 2002-04-10 |
| WO2000051399A1 (en) | 2000-08-31 |
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