CN1549655A - Ceramic heater - Google Patents
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- CN1549655A CN1549655A CNA2004100432783A CN200410043278A CN1549655A CN 1549655 A CN1549655 A CN 1549655A CN A2004100432783 A CNA2004100432783 A CN A2004100432783A CN 200410043278 A CN200410043278 A CN 200410043278A CN 1549655 A CN1549655 A CN 1549655A
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Abstract
A ceramic heater is featured as that heater which is formed by sintered metal granules and metal oxide if necessary is set on surface or in internal of ceramic base plate structured by nitride ceramic or carbide ceramic. In addition, paste made of mixed metal granules and metal oxide is used as electric conducting paste.
Description
The application be that June 9, application number in 1999 are 99800862.1 the applying date, denomination of invention divides an application for the patent of invention of " ceramic heater, its manufacture method and be used for the conductive paste of calandria ".
Technical field
The present invention relates to the desiccant ceramic heater of a kind of semi-conductor industry, particularly a kind of thin and light ceramic heater of temperature control that helps, the conductive paste that the heating element of its manufacture method and formation heater is used.
Background technology
Generally coating corrosion resist on silicon wafer corrodes it then, thereby makes general semiconductor product.In this case, should be after coating, drying coated photosensitive resin to silicon wafer surface.About drying means, generally be that the silicon wafer that scribbles resin is placed on the heater, heating then.
As for this heater, generally be that calandria is fixed on the aluminium substrate back side.Yet this metal heater has problem as described below.
That is, the substrate of heater self is a metal, makes the thickness of substrate should be fabricated into about 15mm.Because the thermal expansion meeting that heating causes produces strain in metal sheet, therefore, place the wafer on the metallic plate can break or perk.Therefore, the problem of common metal heater is a Heavy Weight, and volume is big.
In addition, be added on voltage and current on the calandria, the temperature of control substrate, heater heats silicon wafer by adjusting.Yet the problem of this method is, because hickness of metal plate, the temperature of heater substrate can not be caught up with the variation of voltage or electric current very soon, and the temperature control characteristic is poor.
Summary of the invention
Main purpose of the present invention provides a kind of thin and light heater and manufacture method thereof of temperature control of carrying out easily.
Another purpose of the present invention provides a kind of conductive paste that calandria has excellent heat generation characteristic that is used for.
The problems referred to above that comprise in the routine techniques are checked result, the inventor notice can be with ceramic material with excellent heat conductivity especially nitride ceramics or carbide ceramics, replaced metal such as aluminium for example to make the substrate of heater.Find, this ceramic substrate even warpage or strain can not take place being prepared into Bao Shiye, and can easily carry out temperature control fast, particularly, being added on voltage on the calandria or electric current by change when carrying out temperature control, has excellent response performance.
In addition, the inventor finds that also the conductive paste of containing metal particle generally has the character that almost can not adhere on nitride ceramics or the carbide ceramics, but when adding metal oxide in this conductive paste, by the sintering of metallic particles, can improve adhesiveness.
Based on above-mentioned cognition, made the present invention, it is constructed as follows:
The present invention is a kind of ceramic heater, comprises the ceramic substrate that is made of nitride ceramics or carbide ceramics and is arranged at its lip-deep calandria.
Calandria better is to be arranged to one be partially embedded in ceramic substrate.
Calandria better is that the sintered body by metallic particles constitutes.
Calandria better is by metallic particles and is selected from that at least a metal oxide constitutes in lead oxide, zinc oxide, silica, boron oxide, aluminium oxide, yittrium oxide and the titanium oxide.
As for metallic particles, better be to adopt in noble metal, lead, tungsten, molybdenum and the nickel one or more.
Calandria better is to be coated with non-oxidizing metal level on its surface.
Calandria better is to have section shape to be the section shape of 10-10000 than (thickness of the width/calandria of calandria).
It is characterized in that section shape is arranged in the ceramic substrate that is made of nitride ceramics or carbide ceramics for the flat calandria of 10-10000 than (thickness of the width/calandria of calandria).
The present invention is a kind of ceramic heater, comprise the ceramic substrate that constitutes by nitride ceramics or carbide ceramics, be arranged at the flat calandria in it, wherein the position that is provided with of calandria is the position of departing from the center of substrate on its thickness direction, and is heating surface away from the face of calandria.This heater better is the feature with above-mentioned 2-8 bar.
Calandria better is that the sintered body by metallic particles or conductivity ceramics constitutes.
Calandria better is tungsten, molybdenum, tungsten carbide or molybdenum carbide.
The degree of eccentricity of calandria better is to greater than 50% but less than 100% position from the heating of substrate face.
The calandria section shape better is 10-10000 than (thickness of the width/calandria of calandria).
The invention allows for a kind of method of making ceramic heater, may further comprise the steps at least (1)-(3).
Step (1) sintered nitride ceramic powders or carbide ceramics powder form the substrate that is made of nitride ceramics or carbide ceramics;
Step (2) printing conductive cream on substrate; And
Step (3) is by the heat-agglomerating conductive paste, thereby forms calandria on the surface of ceramic substrate.
Better adopt the non-oxide metal of plating on the surface of gained calandria, thereby form the step of metal coating, as the subsequent step of step (3).
Better be to adopt the compound of metallic particles and metal oxide as the used conductive paste of step (2).
In addition, the invention allows for a kind of method of making ceramic heater, may further comprise the steps at least (1)-(4).
Step (1) is with nitride ceramics powder or carbide ceramics powder forming, thus the green sheet that formation is made of nitride ceramics or carbide ceramics;
Step (2) on the green sheet surface that constitutes by nitride ceramics or carbide ceramics, a type metal particle conductive paste, or the printing and the mixture of its metal oxide;
Step (3) on the other green sheet that one or more utilizations and step (1) same treatment obtain, the stacked green sheet that is printed with conductive paste; And
Step (4) is by heating sintering green sheet and conductive paste under pressure.
Better be, the green sheet of utilizing the processing identical to obtain with step (1) stacked in the green sheet of in step (2), having printed conductive paste upside and during downside, the quantity of green sheet ratio is adjusted to 1/1-1/99 up and down.
In addition, the invention allows for a kind of conductive paste that is used for the calandria of ceramic heater, comprise metallic particles and metal oxide.
As for metallic particles, better be with in noble metal, lead, tungsten, molybdenum and the nickel one or more.
About metal oxide, better be to adopt in lead oxide, zinc oxide, silica, boron oxide, aluminium oxide, yittrium oxide and the titanium oxide one or more.
As for conductive paste, more handy mixing is greater than 0.1wt% but less than the metal oxide of 10wt% and the cream of metallic particles formation.
The average particle size particle size of metallic particles better is the 0.1-100 micron.
Metallic particles better is the mixture of sheet shape particle or spheric granules and sheet shape particle.
Description of drawings
Fig. 1 is the plane graph of ceramic heater of the present invention;
Fig. 2 is a profile of showing the user mode of ceramic heater of the present invention;
Fig. 3 is a diagrammatic sketch of showing the manufacture method of ceramic heater of the present invention;
Fig. 4 show to connect end pin and diagrammatic sketch as the state in the hole of through hole;
Fig. 5 is a diagrammatic sketch of showing the another kind of manufacture method of ceramic heater of the present invention;
Fig. 6 is the diagrammatic sketch of a manufacture method again of showing ceramic heater of the present invention.
Embodiment
Ceramic heater of the present invention is a kind of like this heater, employing is by the ceramic substrate of insulative nitride pottery or carbide ceramics, calandria is formed on the surface of ceramic substrate by printing, its another surface is used as heating surface, and heating is provided with semiconductor products such as for example silicon wafer thereon.
In ceramic heater of the present invention, the calandria with flat section shape can be arranged at the inside (being sandwiched in therebetween) of ceramic substrate, and wherein the calandria center of departing from the substrate thickness direction is provided with, away from the face of calandria as heating surface.
The thermal coefficient of expansion that constitutes the nitride ceramics of substrate or carbide ceramics is littler than metal, has even can not heat the warpage that causes or the character of distortion being prepared into Bao Shiye.Therefore, the substrate of heater can be prepared into thin and light.
In addition, the high and thick degree of this ceramic substrate thermal conductivity is thin, so the surface temperature of substrate can be caught up with the variations in temperature of calandria fast.That is, when changing the temperature of calandria by change voltage or electric current, the surface temperature of ceramic substrate can follow this variation closely and change.
In ceramic heater of the present invention, the substrate face opposite with the side of facing calandria is heating surface, or be heating surface away from the substrate face that departs from the calandria that substrate thickness direction center is provided with, so the heat propagation of spreading on whole substrate is even and rapid, thereby can control the distribution of temperature in the heating surface that limits by the calandria figure, therefore, heating-up temperature is evenly distributed.
About this point, United States Patent (USP) 5643483 discloses a kind of technology, a surface roughening of quartz substrate, and with platinum-palladium cream coating, forms calandria, and wafer is positioned over the substrate surface opposite with the calandria that is used to heat.In addition, United States Patent (USP) 5668524 discloses and a kind ofly has been furnished with the ceramic heater of the embedding chuck wherein of heater.In addition, United States Patent (USP) 5566043 discloses a kind of by the calandria of thermal decomposition graphite formation is positioned over the heater that forms on the surface of boron nitride substrate.
Yet, in United States Patent (USP) 5643483, using quartz substrate, calandria is made of platinum-palladium cream, but the oxide that limits among the present invention do not mix with cream, unless feasible substrate roughening, otherwise can not form calandria.
In the United States Patent (USP) 5668524, the not eccentric setting of calandria does not have concrete shape yet, does not compare etc. so disclose its shape.Therefore, the temperature homogeneity on the heating surface is very poor.
In United States Patent (USP) 5566043, the calandria that adopts thermal decomposition graphite to constitute makes that self burns out calandria when being heated to more than 500 ℃ in air, and therefore the temperature range of using is limited.
The present invention is different from above-mentioned routine techniques fully.
Among the present invention, ceramic substrate better is thick about 0.5-5mm.Because the too thin then substrate of thickness is frangible.
About nitride ceramics, wish to use at least a metal nitride pottery that is selected from aluminium nitride, silicon nitride, the titanium nitride etc. as the material of ceramic substrate.On the other hand, about carbide ceramics, wish to use at least a metal carbides pottery that is selected from carborundum, zirconium carbide, titanium carbide, the tungsten carbide etc.In these potteries, aluminium nitride is better.Because the thermal conductivity of aluminium nitride reaches as high as 180W/m.k.
In addition, by metallic particles in the sintering conductive paste or metal oxide particle, form the calandria that is arranged on the ceramic substrate.These particles can be by baking with agglomeration to the surface of ceramic substrate under the heating condition.In addition, sintering processes proceeds to metallic particles or metallic particles and the pottery degree of fusion each other.
Make the temperature of as a whole ceramic substrate 1 owing to need calandria to raise equably, so calandria 2 better is a same heart-shaped figure as shown in Figure 1.Wish the about 1-50 micron of thickness of the calandria 2 of composition, when calandria 2 was formed on the surface of substrate 1, thickness better was the 1-10 micron.On the other hand, when calandria was formed at substrate 1 inside, thickness better was the 1-50 micron.
In addition, wish the wide about 0.1-20mm of calandria, but when calandria 2 was formed on substrate 1 surface, width better was 0.1-5mm, when calandria 2 was formed at substrate 1 inside, width better was 1-20mm.The reason of these restrictions is that resistance value can change with the change of calandria thickness and width, and control is the most effective but above-mentioned scope is to the temperature of calandria.In addition, the resistance value of calandria 2 can and attenuate and becomes bigger with the calandria attenuation.
In addition, when calandria 2 was formed at substrate 1 inside, thickness and width can form greatlyyer.Because when calandria 2 is arranged in the substrate, the distance between heating surface and calandria shortens, and the temperature homogeneity of the heating surface of ceramic substrate 1 reduces, so for even heating heating surface, require to widen the width of calandria 2 self.On the other hand, in the time of in calandria is arranged at substrate, need not to consider and the nitride ceramics of substrate etc. between adhesiveness, so can use for example carbide of refractory metal such as tungsten, molybdenum and tungsten or molybdenum, therefore, resistance value can increase.As a result, the thickness of calandria can thicken, and breaks etc. preventing.
The section of calandria generally is rectangle or ellipse, but wishes it is pancake.Specifically, when calandria was arranged at the inside of ceramic substrate 1, it must be flat.Because flat section shape towards the heating surface heat radiation, therefore, can cause Temperature Distribution easily hardly in heating surface.
Wishing that calandria 2 section shapes are about 10-10000 than (calandria width/calandria thickness), better is 50-5000.When the shape ratio was adjusted in the above-mentioned scope, the resistance value of calandria 2 can increase, and simultaneously, can guarantee the temperature distribution evenness in the heating surface.
On being arranged at ceramic substrate 1 surface or the thickness of the calandria 2 of its inner composition when being constant, little if shape, then arrives the heat transfer quantitative change of substrate heating surface than little, heating surface is identical with the heat distribution of the calandria of composition.On the contrary, if shape than big, has only the temperature of part on the calandria center of composition to uprise, final on heating surface, form with the composition calandria in identical heat distribution.Consider this Temperature Distribution, the shape of wishing calandria 2 sections than (calandria width/calandria thickness) in the 10-10000 scope.
This is because when the shape ratio of calandria 2 forms 50-5000, can take place hardly because the be full of cracks that thermal shock causes or peel off.
In addition, when calandria 2 was formed at ceramic substrate 1 inside, the shape ratio can form greatlyyer.Yet when forming calandria 2 in inside, the distance between heating surface and calandria shortens, and the uniformity of surface temperature reduces, so calandria self must be a flat pattern.
In the present invention, when calandria 2 is arranged at ceramic substrate 1 inside, calandria can be eccentric in the position that is provided with of thickness direction, but owing to will prevent the Temperature Distribution of heating surface, and the warpage that can control ceramic substrate takes place, and is to greater than 50% but less than 100% position from substrate surface (heating surface) so wish the degree of eccentricity.Better be 55-95%.
In addition, when calandria 2 was formed at ceramic substrate 1 inside, the layer that forms calandria can be divided into multistage.In this case, wish to form the figure of layering,, form a kind of state thus, when heating surface is seen, all formed complete figure in any layer so that make them complimentary to one another.For example, have a kind ofly the upper and lower to be set, make the structure of as a whole full graphics with formation by the grid figure.
In addition, when calandria 2 is arranged on the surface of ceramic substrate 1, wish that the part (bottom) of calandria is embedded in the ceramic substrate.The set-up mode of this calandria can be realized the improvement of calandria resistance control and simultaneously to the adhering improvement of ceramic substrate.
Introduce the conductive paste that is used on ceramic substrate, forming calandria below.Conductive paste normally guarantee the metallic particles of conductivity or conductivity ceramics or with the mixture of resin, solvent, tackifier etc.
About metallic particles, can use to be selected from noble metal (gold, silver, platinum, palladium), lead, tungsten, molybdenum and the nickel one or more.These metals are difficult for oxidized, show as quite heat-resisting.About conductivity ceramics, can constitute by in the carbide that is selected from tungsten or molybdenum etc. one or more.
The particle size of wishing these metallic particles or conductivity ceramics is the 0.1-100 micron.In particle size too hour, oxidation takes place easily, and when too big, almost can not sintering, and resistance value becomes big.
The metallic particles that can use sphere, sheet shape or sphere and sheet shape to mix.Specifically, when being shaped as sheet shape, following metal oxide remains between metallic particles easily, and the adhesiveness between calandria and nitride ceramics etc. improves.
About being used for the resin of conductive paste, better be epoxy resin, phenolic resins etc.About solvent, can use isopropyl alcohol etc.Tackifier can use cellulose etc.
In addition, outside the metallic particles, can also comprise metal oxide in the conductive paste, this metal oxide can form the mixed sintered body of metallic particles and this metal oxide effectively as calandria.That is, when metal oxide was clipped between nitride ceramics or carbide ceramics and metallic particles, adhesiveness can improve.Although it is unclear to improve adhering reason, but there are some oxide-films on the surface of metallic particles or on the surface of nitride ceramics or carbide ceramics a little, show compatibility with metal oxide according to this oxide-film of conjecture, be integral with it easily, therefore can by this oxide with adhering metal particle on nitride ceramics or carbide ceramics.
About metal oxide, can be with being selected from lead oxide, zinc oxide, silica, boron oxide, aluminium oxide, yittrium oxide and the titanium oxide one or more.These oxides can improve the adhesiveness between metallic particles and nitride ceramics or carbide ceramics, can not increase the resistance value of calandria simultaneously.
The addition of wishing metal oxide is that the 0.1-of metallic particles is less than 10wt%.When this measures less than 0.1wt%, can not get additive effect, when this amount was not less than 10wt%, the resistance value of calandria 2 was too big.
In addition, the mixing ratio of wishing these metal oxides is adjusted to when the total amount of metal oxide is 100wt%, lead oxide is 1-10wt%, silica is 1-30wt%, and boron oxide is 5-50wt%, and zinc oxide is 20-70wt%, aluminium oxide is 1-10wt%, yittrium oxide is 1-50wt%, and titanium oxide is 1-50wt%, and its total amount is no more than 100wt%.These scopes are effective especially for the adhesiveness that improves between metallic particles and nitride ceramics.
So the 0.1-that is adjusted to each metallic particles at the addition of metal oxide is during less than 10wt%, the face resistance of calandria can form 1-45 milliohm/.When face resistance becomes too big, too big with respect to institute's making alive heat generation amount, when calandria being arranged on the ceramic substrate surface, be difficult to control, in addition, when the amount of metal oxide was not less than 10wt%, face resistance surpassed 50 milliohms/, and heat generation amount is too big, temperature control is difficult to, and the uniformity of Temperature Distribution reduces in the heater.
Although considered that unless face resistance is not less than 50 milliohms/ (JP-A-4-300249) otherwise the resistive element of heater is inappropriate, but among the present invention, make face resistance be not more than 45 milliohms/ on the contrary and help temperature control, and can guarantee the uniformity of Temperature Distribution.
About another embodiment of the present invention, wish to cover the surface of calandria with metal level.Because as mentioned above, calandria is the sintered body of metallic particles, and in the time of in being exposed to air, oxidation easily changes resistance value.Can prevent this oxidation by the surface that covers the metallic particles sintered body with metal level now.Wish that metal layer thickness is about 0.1-10 micron.Because this scope can prevent the calandria oxidation, do not change the resistance value of calandria simultaneously.
Being coated in the lip-deep metal of metallic particles sintered body can the right and wrong oxidized metal.For example, can be to be selected from gold, silver, palladium, platinum and the nickel one or more.Wherein, nickel is better.Owing to generally need calandria to have to be used to connect the terminal of power supply, and this terminal is fixed on the calandria by scolder, and nickel has the effect that prevents the solder heat diffusion.About splicing ear, can use the end pin (terminal pin) that constitutes by the kovar teleoseal.
Yet when calandria was arranged at ceramic substrate inside, the calandria surface was not oxidized, so need not to cover.
About scolder, can constitute by for example solder alloys such as silver-lead, lead-bismuth, bismuth-Xi.The thickness of solder layer is just enough in the scope of 0.1-50 micron, can guarantee to use the connection of scolder.
Among the present invention, shown in Fig. 5 (d), if necessary, at ceramic substrate 1 embedded set thermocouple 61.Thermocouple 61 is measured the temperature of ceramic substrates 1, and according to measurement data regulation voltage and electric current, thereby controls the temperature of the heating surface of ceramic substrate 1 easily and accurately.
Fig. 2 is a part sectioned view of showing the user mode of ceramic heater of the present invention.Numeral 3 is end pins, and numeral 4 is metal (Ag-Pb) particle sintered bodies, and numeral 5 is metal (Ni) cover layers, and calandria 2 constitutes by 4 and 5.In addition, numeral 6 is solder layers, and end pin is fixed by solder layer.
In addition, be formed with a plurality of through holes 8 in the ceramic substrate 1, the supporting pin 7 that is used for semiconductor wafer is inserted in through hole 8, and semiconductor wafer 9 is fixed in the top of the pin 7 that is projected on the ceramic substrate 1, and is adjacent with it or have slightly at interval.In this case, semiconductor wafer 9 is sent on the transport sector (not shown), or by promoting and falling supporting pin 7 and take off semiconductor wafer 9 from transport sector.
Introduce the method that the present invention makes ceramic heater below.
A. on the ceramic substrate surface, form the situation (Fig. 2) of calandria.
Sintering insulated nitride ceramics of step (1) or insulation carbide ceramics powder, thereby the plate body (ceramic substrate) of formation nitride ceramics or carbide ceramics.
In this step, for example utilize spraying-seasoning etc., with the pottery of aluminum nitride and other nitride for example or for example carbide ceramics such as carborundum powder or form particle with the mixed-powder of sintering aid such as for example yittrium oxide and adhesive if desired, and resulting granules is positioned in mould etc., by press molding is plate shape, forms the green sheet body.
If desired, form through hole 8 and recess 62 in the green sheet body, said through hole 8 is used to insert the supporting pin 7 of semiconductor wafer, embedding thermocouple 61 in the recess 62.
Then, by heating and calcining, sintering green sheet body forms the ceramic wafer body.When heating and calcining, pressurization is formed for the atresia ceramic substrate of heater.This heating and calcining can be carried out more than sintering temperature, but for nitride ceramics or carbide ceramics, better are 1000-2500 ℃.
The conductive paste of printing containing metal particle on the surface of the ceramic wafer body that step (2) obtains in step (1) (heater substrate or ceramic substrate), thus metallic particles layer 4 formed.
In this step, utilize methods such as for example silk screen printing, the conductive paste that is made of metallic particles, resin and solvent is printed on given position.Why to be the concentric circles figure of wishing accurately to form as shown in Figure 1 that is used to form calandria 2, so that heat whole ceramic substrate with even temperature by the reason of printing coating electrically conductive cream.
In addition, the section shape of calandria is a rectangle as pedestal, and wishes it is flat section shape.
Step (3) sintering under heating condition is formed on metallic particles layer on the ceramic substrate by printing, thereby forms calandria 2 on the surface of ceramic substrate 1.
The metallic particles layer of the printing formation of conductive paste is passed through in heating and calcining, thereby removes resin and solvent, and sintered metal particle (the heating and calcining temperature is 500-1000 ℃).About this point, for example, when adding metal oxide in conductive paste, metallic particles, ceramic wafer body and metal oxide are integrated by sintering, so the adhesiveness of calandria and ceramic wafer body improves.
(4) in addition, if desired, on the surface of metallic particles layer 4, form metal cladding.This processing can be undertaken by metallide, electroless plating, sputter etc., but considers batch process, and electroless plating is the most suitable.
(5) fixing end pin 3 on the end of the figure of the calandria that obtains like this is used for being connected to power supply by scolder.
B. under the situation in calandria is formed at ceramic substrate (Fig. 3).
(1) ceramic powders such as nitride ceramics or carbide ceramics and adhesive and solvent obtain green sheet 31.
About ceramic powders, available aluminium nitride, carborundum etc. if desired, can add for example sintering aid such as yittrium oxide.About adhesive, hope is at least a in acryloid cement, ethyl cellulose, butyl fiber and the polyethylene.About solvent, wish to adopt α-terpineol and ethylene glycol.
Utilize the scraping blade method to be shaped and mix the cream that they obtain, form green sheet 31.If desired, in the green sheet that obtains like this, can be formed for inserting silicon wafer supporting pin 7 through hole 8 or be used for the recess 62 of embedding thermocouple 61.Through hole 8 or recess 62 form by methods such as perforation.
The thickness of green sheet is about 0.1-5mm.
(2) then, on green sheet the type metal stratum granulosum as calandria.
Metallic particles layer 4 as calandria forms by utilizing conductivity ceramics type metal cream or conductive paste.
This cream contains metallic particles or conductivity ceramics particle.About metallic particles, tungsten or molybdenum the best, about the conductivity ceramics particle, carbide the best of tungsten or molybdenum.Because they hardly can be oxidized, and can reduce thermal conductivity hardly.
The average particle size particle size of tungsten particle or molybdenum particle is the 0.1-5 micron.In this size too greatly or too hour, all be difficult to printing conductive cream.About conductive paste, preferably utilize and mix tungsten cream or the molybdenum cream that 85-97 part metallic particles by weight or conductivity ceramics particle, 1.5-10 part are selected from least a solvent preparation that at least a adhesive in acryloid cement, ethyl cellulose, butyl fiber and the polyethylene and 1.5-10 part is selected from α-terpineol and ethylene glycol.
(3) then, be layered in step (2) and printed another green sheet 31 that green sheet 31 method identical with step (1) with utilization of calandria 2 obtains.
In this illustrative embodiments, go up stacked 37 at metallic particles layer 4 (heating surface side), stacked 17 at opposite side.That is, by making upside (heating surface side) (2) that a plurality of green sheet (1) are laminated in calandria, the formation position of calandria 2 is formed in thickness direction off-centre in the stacked printing green sheet of Duoing of downside than these a plurality of green sheet.Hope is by stacked a large amount of green sheet with same thickness, and the ratio that makes upper and lower sides is 1/1-1/99.Thereby, at the stacked 20-50 sheet of upside, at the stacked 5-20 sheet of downside.
(4) by heating and pressure sintering green sheet and conductive paste.Heating-up temperature is 1000-2000 ℃, adds to be pressed in the inert gas atmosphere at 100-200kg/cm
2Carry out under the condition.About inert atmosphere, can use argon, nitrogen etc.
At last, on a part, print soldering paste,, after this, place end pin 3, and fix it by reflux with fixing end pin 3.The heating-up temperature of Reflow Soldering better is 200-500 ℃.In addition, if desired, can immersion thermocouple.
Example
(example 1) heater is made of aluminium nitride ceramic substrate
(1) utilize spray drying process, 100 parts of aluminium nitride powders (average particle size particle size is 1.1 microns), 4 parts of yittrium oxide (average particle size particle size is 0.4 micron), 12 portions of acryloid cements and pure mixture are made nodular powder by weight.
(2) this nodular powder is put into mould, and be configured as flat, obtain the green sheet body.Punch with being drilled on this green sheet, be formed for inserting the through hole 8 of supporting pin of semiconductor wafer and the recess (not shown) of embedding thermocouple.
(3) at 200kg/cm
2Pressure under, at this green sheet body of 1800 ℃ of hot pressing, obtain the nitrogenize aluminium sheet body of thick 3mm.It is cut into the disk that diameter is 210mm, forms ceramic laminate body (ceramic substrate) 1.
(4) silk screen printing conductive paste on the ceramic substrate 1 that in (3) bar, obtains.The figure of printing is a concentric circles figure as shown in Figure 1.The commodity Solvest PS 603D that adopts Tokuriki Kagaku Kenkyusho to make makes conductive paste, is used for forming through hole at printed circuit board (PCB).This conductive paste is silver-lead plaster, contains the oxide as lead oxide, zinc oxide, boron oxide, silica and aluminium oxide (weight ratio is 5/55/10/25/10) mixture of 7.5wt% in every part of silver.In addition, silver employing average particle size particle size is 4.5 microns a sheet shape.
(5) heat and calcine the ceramic substrate that is printed with conductive paste, the silver in the sintering conductive paste and plumbous, and roasting ceramic substrate 1 down at 780 ℃.Silver-plumbous figure sintered body 4 thick 5 microns, wide 2.4mm, face resistance are 7.7 milliohms/.
(6) ceramic substrate 1 of (5) bar is immersed in the aqueous solution of ammonium chloride of the boric acid of sodium acetate, 8g/l of sodium hypophosphite, the 12g/l of the nickelous sulfate that comprises 80g/l, 24g/l and 6g/l, the nickel dam of 1 micron of deposition of thick on the surface of silver-plumbous sintered body 4, thus calandria 2 formed.
(7) utilize silk screen print method, printed silver on the terminal standing part of guaranteeing to be connected with power supply-lead welding cream forms solder layer (Tanaka Kinzoku K.K manufacturing) 6.Then, kovar teleoseal end pin 3 is set on solder layer 6, heats down at 420 ℃ and reflux, end pin 3 is fixed on the surface of calandria 2.
(8) embeddingly be used for temperature controlled thermocouple (not shown), obtain heater 100 (Fig. 1 and 2).
The heater that (example 2) silicon carbide ceramics substrate constitutes
Remove adopting average particle size particle size is 1.0 microns silicon carbide powder, and sintering temperature is 1900 ℃, 1500 ℃ down the calcining surface formed thick 1 micron SiO in 2 hours from the teeth outwards
2Outside the layer, repeat and example 1 essentially identical step.
(example 3)
Heater about example 1 and 2, the temperature-responsive and the hot strength of the heating surface of ceramic substrate when the power supply of measurement change calandria 2 or electric current, that is, and when giving each heater making alive, observe the variations in temperature in example 1 heater 0.5 second, observe the variations in temperature in example 2 heaters 2 seconds.On the other hand, the hot strength of calandria 2 is respectively: 3.1kg/mm in example 1 heater
2, 3kg/mm in example 2 heaters
2
(example 4) calandria is arranged at its inner heater (Fig. 3,5)
(1) utilizes scraper, being shaped by weight, (Tokuyama company makes 100 parts of aluminium nitride powders, average particle size particle size is 1.1 microns), 4 parts of yittrium oxide (average particle size particle size is 0.4 micron), 11.5 portions of acryloid cements, 0.5 part of dispersant and 53% 1-butanols and the mixture of ethanol by weight, obtain the green sheet 31 of thick 0.47mm.
(2) under 80 ℃ with this green sheet 31 dry 5 hours, by perforation, be formed for inserting the through hole and the through hole 38 that is used for being connected between calandria and end pin of the supporting pin of semiconductor wafer, their diameter is respectively 1.8mm and 3.0mm and 5.0mm.
(3) mix by weight that 100 parts of average particle size particle size are 1 micron tungsten carbide particle, 3.0 portions of acryloid cements, 3.5 parts of α-terpineols and 0.3 part of dispersant, preparation conductive paste A.
In addition, mixing 100 parts of average particle size particle size by weight is 3 microns tungsten carbide particle, 1.9 portions of acryloid cements, 3.7 parts of α-terpineols and 0.2 part of dispersant, preparation conductive paste B.
Utilize silk screen print method with graphic form printing conductive cream A on green sheet 31.The figure of printing is concentric circles as shown in Figure 1.In addition, filled conductive cream B in through hole 38 is to connect end pin.
In addition, go up stacked 37 green sheet 31 that do not have printing conductive cream A at upside (heating surface), in stacked 17 green sheet 31 of downside, at 80kg/cm
2Pressure under, with they integrators, obtain lamination (Fig. 3) under 130 ℃ the temperature.
(4) under 600 ℃ of temperature, in the nitrogen, lamination was deoiled 5 hours, and at 150kg/cm
2Pressure under, 1890 ℃ of hot pressing 3 hours, obtain the nitrogenize aluminium sheet body of thick 3mm.It is cut into the disk that diameter is 230mm, so that the ceramic substrate 51 (Fig. 5 (a)) with the wide calandria of 6 micron thickness and 10mm to be provided.
(5) with the ceramic substrate 51 in boart boart buff polishing (4) bar, mask is set thereon, carries out blasting treatment, be formed for holding the hole 62 (Fig. 5 (d)) of thermocouple with bead.
(6) in addition, enlarge the surface portion of through hole 38, form recess 48 as shown in Figure 4, in this recess 48, provide the gold solder that constitutes by the Ni-Au alloy, and 700 ℃ of following reflux, to connect kovar teleoseal end pin 60 (Fig. 5 (c)).
In addition, utilize recess 48 to make the supported at three point that connects into of end pin 60, to guarantee the connection reliability of end pin 60.
(7) embeddingly in hole 62 a plurality ofly be used for temperature controlled thermocouple 61, thereby obtain ceramic heater (Fig. 5 (d)).
(comparative example) aluminium sheet heater
Use the nickel-chromium silk that is supported by silicone rubber to make calandria, they are clipped between the aluminium sheet and supporting bracket of thick 15mm, and by bolt, form heater.After voltage is added on this heater, needed 24 seconds just can observe variations in temperature.
(comparative example 2) aluminium oxide heater
Remove the mixture that will comprise 100 parts of alumina powders of weight meter (1.0 microns of average particle size particle size), 12 portions of acryloid cements and alcohol and make granularly, and place mould, be configured as plate shape, thereby form green sheet, then at 200kg/cm with spray drying process
2Pressure under, 1200 ℃ of these green sheet of hot pressing, thereby obtain outside the alumina substrate of thick 3mm, basic repeat the program identical with example 1.
In addition, 100 parts of average particle size particle size are 3 microns tungsten particle, 1.9 portions of acryloid cements, 3.7 parts of α-terpineols and 0.2 part of dispersant by mixing by weight, preparation conductive paste, and printing.Be printed with the ceramic substrate of conductive paste, sintered tungsten at 1000 ℃ of following heating and calcinings.
(example 5)
It is not flat removing calandria, but section is outside 20 micron thickness * 20 micron wide square (the shape ratio is 1), repeats the program identical with example 4 substantially.
(example 6)
Remove printing condition and change, and calandria is not flat, but section is outside 5 micron thickness * 72 mm wides (the shape ratio is 12000), repeat the program identical substantially with example 4.
(example 7)
Remove in stacked 24 green sheet of the green sheet upside that is printed with conductive paste, in stacked 25 green sheet of its downside, and calandria is arranged at outside the ceramic substrate center, repeats the program identical with example 4 substantially.
(example 8)
The conductive paste that has following component except that preparation replaces the Solvest PS 603D, repeats the program identical with example 1 substantially.
100 parts of silver powder shape beads by weight, average particle size particle size is 5.0 microns
7.5 parts of metal oxides (weight ratio of lead oxide/zinc oxide/silica/boron oxide/aluminium oxide is 5/55/10/25/5) by weight
Face resistance 4 milliohms/
(example 9)
(1) utilize spray drying process, 100 parts of aluminium nitride powders (average particle size particle size is 1.1 microns), 4 parts of yittrium oxide (average particle size particle size is 0.4 micron), 12 portions of acryloid cements and pure mixture are made granular by weight.
(2) this nodular powder is put into mould, and be configured as flat, obtain green sheet.Punch with being drilled on this green sheet, be formed for inserting the through hole of supporting pin of semiconductor wafer and the base apertures of embedding thermocouple.
(3) at 200kg/cm
2Pressure under, 1800 ℃ of these green sheet of hot pressing, obtain the aluminium nitride board substrate of thick 3mm.It is cut into the disk that diameter is 210mm, forms ceramic substrate 1.
In addition, on ceramic substrate 1, metal mask is set, and is that 1 micron alumina powder carries out blasting treatment, form wide 2.4mm and dark 6 microns groove in the position that forms calandria with diameter.
(4) silk screen printing conductive paste on the groove of the ceramic substrate 1 that obtains in step (3) forms the metallic particles layer.The figure of metallic particles layer is a concentric circles figure as shown in Figure 1.The commodity Solvest PS 603D that makes with Tokuriki Kagaku Kenkyusho makes conductive paste, is used for forming through hole at printed circuit board (PCB).This conductive paste is silver-lead plaster, contains the oxide as lead oxide, zinc oxide, boron oxide, silica and aluminium oxide (weight ratio is 5/55/10/25/5) mixture of 7.5wt% in every part of silver.In addition, silver adopt average particle size particle size be 4.5 microns tablet.
(5) heat and calcine the ceramic substrate that provides metallic particles down at 780 ℃, the silver in the sintered metal particle layer (conductive paste) and plumbous, and roasting is to ceramic substrate 1.Thick 5 microns of silver-plumbous figure sintered body 4 figures, wide 2.4mm, face resistance are 7.7 milliohms/.
(6) ceramic substrate of (5) bar is immersed in the aqueous solution of ammonium chloride of the boric acid of sodium acetate, 8g/l of sodium hypophosphite, the 12g/l of the nickelous sulfate that comprises 80g/l, 24g/l and 6g/l, the nickel dam 5 of 1 micron of deposition of thick on the surface of silver-plumbous sintered body 4, thus calandria formed.
(7) utilize silk screen print method, printed silver on the terminal standing part of guaranteeing to be connected with power supply-lead welding cream forms solder layer (Tanaka Kinzoku K.K manufacturing) 6.Then, kovar teleoseal end pin is set on solder layer 6,420 ℃ down heating reflux, end pin is fixed in (see figure 6) on the surface of calandria 2.
In this example, calandria is embedded in the ceramic substrate, but exposes from its surface, shown in Fig. 6 (a).In addition, calandria can partly be embedded in the ceramic substrate, and a part is exposed state, shown in Fig. 6 (b).
In this example, the same response time, temperature difference and the hot strength measured with example 1 and 8.The results are shown in table 1.
(comparative example 3)
Except that in Solvest PS 603D, adding lead oxide and zinc oxide so that the amount of metal oxide is adjusted to the 10wt%, the program that basic repetition and example 1 are identical.The face resistance of gained calandria is 50 milliohms/.
In addition, routine 1-8 (except the example 3) and comparative example 1-3 were measured behind the making alive up to the time (response time) that confirms variations in temperature.In addition, measurement maximum temperature and minimum temperature of heating surface when surface temperature is 600 ℃ is poor.In addition, to the area inner measuring hot strength (units/2mm) of routine 1-8 at 2mm * 2mm.The results are shown in Table 1.
Table 1
| Response time (second) | Temperature difference (℃) | Hot strength (kg/2mm) | |
| Example 1 | ????0.5 | ????8 | ????12.4 |
| Example 2 | ????2.0 | ????9 | |
| Example 4 | ????1.0 | ????8 | |
| Example 5 | ????1.6 | ????15 | |
| Example 6 | ????0.8 | ????18 | |
| Example 7 | ????0.7 | ????18 | |
| Example 8 | ????0.7 | ????18 | ????6.0 |
| Example 9 | ????0.8 | ????9 | ????24.0 |
| Comparative example 1 | ????24 | ????15 | |
| Comparative example 2 | ????40 | ????22 | |
| Comparative example 3 | ????0.8 | ????15 |
As mentioned above, ceramic heater of the present invention is not only thin but also light and practical, is specially adapted to heating of semi-conductor industry field and drying of semiconductor product.
In addition, in ceramic heater of the present invention, make ceramic substrate with nitride ceramics or carbide ceramics, and thin thickness, so change the temperature-responsive excellence of heating surface with respect to voltage or electric current, and carry out temperature control easily.And, the uniformity of temperature profile of heating surface, and can the efficient drying semiconductor product.
Claims (7)
1. a ceramic heater comprises the ceramic substrate that is made of nitride ceramics or carbide ceramics and is arranged at its lip-deep calandria.
2. according to the ceramic heater of claim 1, wherein calandria is arranged to one and is partially embedded in ceramic substrate.
3. according to the ceramic heater of claim 1, wherein calandria is made of the sintered body of metallic particles.
4. according to the ceramic heater of claim 1, wherein calandria is made of the mixed sintering body of metallic particles and metal oxide.
5. according to claim 1,2,3 or 4 ceramic heater, wherein metallic particles adopts and is selected from noble metal, lead, tungsten, molybdenum and the nickel one or more.
6. according to claim 1,2,3,4 or 5 ceramic heater, wherein be coated with non-oxidizing metal level on the calandria surface.
7. according to claim 1,2,3,4,5 or 6 ceramic heater, wherein calandria has section shape and is the section shape of 10-10000 than (thickness of the width/calandria of calandria).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100432783A CN1549655A (en) | 1999-06-09 | 1999-06-09 | Ceramic heater |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100432783A CN1549655A (en) | 1999-06-09 | 1999-06-09 | Ceramic heater |
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| CN99800862A Division CN1296724A (en) | 1999-06-09 | 1999-06-09 | Ceramic heater and method for producing the same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102779777A (en) * | 2008-01-08 | 2012-11-14 | 日本碍子株式会社 | Bonding structure |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102779777A (en) * | 2008-01-08 | 2012-11-14 | 日本碍子株式会社 | Bonding structure |
| CN102779777B (en) * | 2008-01-08 | 2015-07-01 | 日本碍子株式会社 | Bonding structure |
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