CN106376107A

CN106376107A - Large-power silicon nitride ceramic heating plate and inner-soft outer-hard manufacturing method thereof

Info

Publication number: CN106376107A
Application number: CN201611042278.0A
Authority: CN
Inventors: 肖毅
Original assignee: Changde Cree New Mstar Technology Ltd
Current assignee: Changde Cree New Mstar Technology Ltd
Priority date: 2016-11-24
Filing date: 2016-11-24
Publication date: 2017-02-01
Anticipated expiration: 2036-11-24
Also published as: CN106376107B

Abstract

The invention relates to a large-power silicon nitride ceramic heating plate and an inner-soft outer-hard manufacturing method thereof. The large-power silicon nitride ceramic heating plate comprises an insulated ceramic plate, heating ceramics, welding ceramics and external leads. The manufacturing method comprises the steps that 1) ball milling, drying, bonding agent adding, draying and sieving are carried out on an insulated ceramic material successively; 2) cold-press molding, drying, sintering and cutting molding are carried out on the insulated ceramic material; 3) heating ceramic powder and welding ceramic powder are added into a bonding agent, the ceramic powder and the bonding agent are mixed, dried, granulated and molded, and then placed into an insulated ceramic body, and the powder, the bonding agent and ceramic body are integrated by integral pressing; 4) wholly hardening and debonding are carried out; and 5) sintering, hardening and modeling are carried out. The large-power silicon nitride ceramic heating plate and the manufacturing method thereof have the advantages that 1) heating is rapid, and temperature control is accurate; 2) heating is very uniform, and heat loss is very low; 3) three types of ceramics are uniformly solid-dissolved, sintered and thus integrated, the quality is high, the possibility of problems is reduced; and 4) welding is very firm.

Description

High-power silicon nitride ceramics heating plate and its manufacture method of hard outside soft inside

Technical field

The present invention relates to silicon nitride ceramics, the i.e. manufacture method of high-power silicon nitride ceramics heating plate and its hard outside soft inside.

Background technology

High-power silicon nitride ceramics heating plate, generally refers to more than 500w, and unit area power is more than 50 watts/cm².

Due to lightweight, small volume, firing rate is fast, power is big, heat consumption is little, heat transfer passs efficiency high, stable at high temperature not The features such as deformation all trades and professions, especially used in electron trade more and more, more and more extensively.

Domestic making silicon nitride ceramics heating plate has following 2 kinds of processes at present:

Method one: tungsten filament is curved spring-like, by the different resistance needing, the spring of different length is placed on silicon nitride material In, compacting, sintering, then weld lead-out wire.As shown in Figure 1.

Method two: prepare silicon nitride flat ceramic base substrate and the tungsten slurry being cast, the mode of tungsten slurry silk screen printing is printed Brush the conductor that heating is formed on silicon nitride flat board base substrate, then answer last layer ceramic body again, sintering forms.As shown in Figure 2.

Method three: " silicon nitride heating sheet and preparation method thereof " of Patent No. 2012100471693, using si₃n₄Powder Carry out the method that casing pressure is integral and then is sintered with calandria powder.

These three processes have the shortcomings that than more serious:

1: on pottery make heating plate, mainly use pottery on smaller area make relatively high power and thermal losses Little device, but the general all very littles of the heating tungsten filament diameter using, in φ 0.4-0.5mm, this thin tungsten filament and pottery Powder sintering can not mix together well, very fragile.

2: ceramic post sintering is polycrystal it is impossible to not have micro- pore, this can be seen that under high power microscope, and tungsten filament is in sky In gas, heating is to be very easy to become fragile blow, and this is the flimsy main cause of ceramic heating flake.

3: the grain shape of ceramic powder is different, diameter 0.4mm about thin tungsten filament at high temperature under high pressure with pottery Porcelain granule is sintered together, the serious damage of tungsten filament, is very easy to fracture of wire in long-term reuse.

4. the heating plate making on pottery curtain coating substrate, due to there being degumming tech, is to make powerful product, pottery Generally alumina material, alumina material thermal shock resistance is poor, can only do low power.

5: because tungsten filament is that the spring-like heater being coiled into different lead is inserted in ceramic powder, spring helical pitch size can not Can control very accurate, cause to heat uneven.

6: tungsten filament spring is added in ceramics, technics comparing is complicated, anthropic factor is larger, actual power change is compared Greatly, wayward.

7: tungsten filament is embedded in pottery, outlet end area very little, welding lead-out wire is difficult very much, and not prison welding is to use The main cause going wrong in journey.

8: because heating tungsten filament is in ceramic body, has uncertainty, resistance variations are big in use, and power is unstable, send out Thermal change is very big.

9. in patent application 2012100471693 " silicon nitride heating sheet and its manufacture method ", have the shortcomings that two big, one It is the component unreasonable allocation of body and calandria；Two is when covering molded, hot zone and not hot zone in body, calandria Powder base all crushed, area and length wayward, the length of hot zone and not hot zone in product, area inaccurate, It is inaccurate that this two shortcomings result in resistance, power also inaccurate it is impossible to be produced in batches.

Content of the invention

In order to overcome that tungsten filament in above-mentioned three kinds of methods is fragile, heating is uneven, be difficult to weld lead-out wire, power unstable The shortcomings of, the manufacture method that the present invention proposes a kind of new high-power silicon nitride ceramics heating plate and its hard outside soft inside.

This high-power silicon nitride ceramics heating plate, with silicon nitride as main raw material(s) it is characterised in that including insulation pottery Porcelain plate, heating ceramic, welding ceramics and external wire, on the median plane of insulated ceramic plates, sintering has the conductive pottery of u shape arrangement Porcelain, the two ends of conductivity ceramics are connected with welding ceramics, and welding ceramics have one side to expose in insulated ceramic plates, are solder side, External wire is welded with solder side.Below this several part is described below respectively:

1st, heating ceramic, is mixed by conductive metal dust and nonconducting non-metal powder, by adjusting metal dust Reach the effect adjusting resistance, electrified regulation with the ratio of non-metal powder, reach the heating power of design.

2nd, insulated ceramic plates, are the big insulated compound potteries of thermal capacity, intensity height, heat shock resistance, heat stability are high.

3rd, welding ceramics, are rapidly transferred to heating ceramic electric energy, and itself does not generate heat thus protecting leading-out terminal temperature Not high, safe wiring.

4th, external wire, metal wire is welded in the exposed surface of welding ceramics it is ensured that outlet is firm, reliable.

This high-power silicon nitride ceramics heating plate, its ceramic heating body is by the ceramic material group of three part different proportions Become, as follows by weight proportion:

1st, insulating ceramic materials: silicon nitride si₃n₄, 91.5-94%；Ytterbium oxide y₂o₃, 1-3%；Aluminium oxide al₂o₃, 0.5- 1.5%；Magnesium oxide mgo, 0.2-0.5%；Lanthanum sesquioxide la₂o₃, 0.5-1%；Hafnium oxide hfo₂, 0.2-0.5%, aluminium nitride aln, 0.5-2%, whole composition weight are 100%.

2nd, heating ceramic material: silicon nitride si₃n₄, 40-50%, the solid solution of titanium carbide and titanium nitride, ti(c, n), 26- 35%；In solid solution, the weight of titanium carbide and titanium nitride is than for 4:6；Molybdenum powder mo, 0.5-3%；Nano nickel ni, 0.5-1.0%；Carbonization Niobium chnb, 0.2%；Whisker carborundum sic, 0.2-0.5%；Molybdenum silicide mosi₂, 0.1-0.2%；Silicon oxide sio₂, 0.1-0.2%； Aluminium oxide al₂o₃, 5-10%, whole composition weight are 100%.

3rd, welding ceramics material: titanium carbide tic, 60-72%；Silicon nitride si₃n₄, 20-30%；Whisker carborundum sic, 0.2- 0.5%；Molybdenum silicide mosi₂, 0.1-0.2%；Aluminium oxide al₂o₃, 5-10%；Silicon oxide sio₂, 0.1-0.2%, whole composition weight For 100%.

The manufacture method of this high-power silicon nitride ceramics heating plate hard outside soft inside is it is characterised in that step is as follows:

First, insulating ceramic materials use nylon tank, silicon nitride si respectively₃n₄Ball carries out ball milling, carries out drying in 72 hours, make to contain after mill The water yield is less than 1%, using pollution-free blender batch mixing, adds bonding agent Polyethylene Glycol peg during batch mixing, its weight accounts for insulating ceramics material The 1-1.5% of material weight, dries, sieve 60 mesh, standby；

2nd, using the particular manufacturing craft being made according to client's part requirements, so that insulating ceramic materials isostatic cool pressing cip is shaped, do Go out insulating powder ceramic body post-drying, after putting into gas pressure sintering stove gps sintering, laser cutting machine cutting cnc is processed into required shape Shape, standby；

3rd, the Polyethylene Glycol peg bonding agent being separately added into respective weight 1-1.5% in heating ceramic powder and welding ceramics powder is mixed Even, dry, pelletize, with isostatic cool pressing cip shape be pressed into lamellar, respectively using particular manufacturing craft molding, be then placed in insulating ceramics In base substrate, overall pressing is integrated；

4th, overall hardening degumming；

5th, put into hot isostatic pressure stove hip stove to sinter, reinforcement, stiffened molding, 1800 DEG C -1820 DEG C of maximum sintering temperature, Pressure: 1500mpa.

This Compound Machining forming process is commonly called as hard outside soft inside technique.

The advantage of this high-power silicon nitride ceramics heating plate is:

1st, global density is in 3.4-3.6g/cm³, wherein heating ceramic density < 5 g/cm³, insulating ceramics density < 3.25 g/cm³, Ceramic heating flake density relatively low, have relatively low thermal capacity, can quickly heat, reach 1000 c need to the time be less than 10 seconds, Temperature control accurately, is that autocontrol temperature provides good condition.

2nd, heating ceramic is sintered to polycrystalline structure, and heating is highly uniform, and thermal losses is very low.

3rd, heating ceramic and the mutually uniform solid solution sintering of insulating ceramics, welding ceramics are integrated, and no interface greatly improves The quality of heating plate, reduces the probability going wrong.

4th, because welding ceramics outlet welding ends is rectangle, solder side is larger, and stock size is 3x1.5mm, therefore welds out Line is very firm.

5th, electric heating body is to send out infrared long-wave radiation heat transfer, and the heat generating ceramic radiation coefficient of the present invention is more than 0.9. And tungsten filament radiation coefficient is only 0.04 hence it is evident that radiations heat energy is little.

When the 6th, sintering, insulating ceramics, heat generating ceramic, welding ceramics interface understand, but can be suitable mutually invade profit, resistance Stable and accurate.

Brief description

Fig. 1 is the structure chart of traditional ceramicses fever tablet one

Fig. 2 is the structure chart of traditional ceramicses fever tablet two

Fig. 3 is the structure chart of the ceramic heating plate of the present invention

In FIG: 1, silicon nitride ceramics, 2, tungsten filament spring, 3, tungsten filament, 4, welding ceramics, 5, external wire；

In fig. 2: 1, tungsten slurry, 2, ceramic idiosome；

In figure 3: 1, insulating ceramics, 2, conductivity ceramics, 3, welding ceramics, 4, solder side, 5, external wire.

Specific embodiment

As follows to the detailed description of the invention below by specific embodiment:

This high-power silicon nitride ceramics heating plate, as shown in Figure 3.Now enumerate three descriptions of product of laboratory manufacture.Its pottery Porcelain calandria is made up of the ceramic material of three part different proportions, as follows by weight proportion:

Embodiment one, cigar lighter, specification 90x5x4mm, 500 watts, 1100 DEG C, it is worked into 1100 DEG C within 10 seconds.

1st, insulating ceramic materials: silicon nitride si₃n₄, 94%；Ytterbium oxide y₂o₃, 1-3%；Aluminium oxide al₂o₃, 0.5-1.5%； Magnesium oxide mgo, 0.2-0.5%；Lanthanum sesquioxide la₂o₃, 0.5-1%；Hafnium oxide hfo₂, 0.2-0.5%, aluminium nitride aln, 0.5- 2%, whole composition weight are 100%.

2nd, heating ceramic material: silicon nitride si₃n₄, 45%, the solid solution of titanium carbide and titanium nitride, ti(c, n), 26-35%； In solid solution, the weight of titanium carbide and titanium nitride is than for 4:6；Molybdenum powder mo, 0.5-3%；Nano nickel ni, 0.5-1.0%；Niobium carbide Chnb, 0.2%；Whisker carborundum sic, 0.2-0.5%；Molybdenum silicide mosi₂, 0.1-0.2%；Silicon oxide sio₂, 0.1-0.2%；Oxygen Change aluminum al₂o₃, 5-10%, whole composition weight are 100%.

3rd, welding ceramics material: titanium carbide tic, 60%；Silicon nitride si₃n₄, 20-30%；Whisker carborundum sic, 0.2- 0.5%；Molybdenum silicide mosi₂, 0.1-0.2%；Aluminium oxide al₂o₃, 5-10%；Silicon oxide sio₂, 0.1-0.2%, whole composition weight For 100%.

The manufacture method of this high-power silicon nitride ceramics heating plate hard outside soft inside, step is as follows:

4th, overall hardening degumming；

Embodiment two, drying sheet, specification 1200x12x4mm, 600 watts, it is worked within 2 seconds 258 DEG C, durability 2 years.Three kinds In the part by weight of ceramic material,

1st, insulating ceramic materials: silicon nitride si₃n₄, 92%；Ytterbium oxide y₂o₃, 1-3%；Aluminium oxide al₂o₃, 0.5-1.5%；Oxidation Magnesium mgo, 0.2-0.5%；Lanthanum sesquioxide la₂o₃, 0.5-1%；Hafnium oxide hfo₂, 0.2-0.5%, aluminium nitride aln, 0.5-2%.

2nd, heating ceramic material: silicon nitride si₃n₄, 45%, the solid solution of titanium carbide and titanium nitride, ti(c, n), 26-35%； In solid solution, the weight of titanium carbide and titanium nitride is than for 4:6；Molybdenum powder mo, 0.5-3%；Nano nickel ni, 0.5-1.0%；Niobium carbide Chnb, 0.2%；Whisker carborundum sic, 0.2-0.5%；Molybdenum silicide mosi₂, 0.1-0.2%；Silicon oxide sio₂, 0.1-0.2%；Oxygen Change aluminum al₂o₃, 5-10%.

3rd, welding ceramics material: titanium carbide tic, 66%；Silicon nitride si₃n₄, 20-30%；Whisker carborundum sic, 0.2- 0.5%；Molybdenum silicide mosi₂, 0.1-0.2%；Aluminium oxide al₂o₃, 5-10%；Silicon oxide sio₂, 0.1-0.2%.

Remaining process conditions is identical with embodiment 1.

Embodiment three, heating plate, specification 150x25x4mm, 800 watts, it is heated to 1000 DEG C within 10 seconds.

In the part by weight of three kinds of ceramic materials,

1st, insulating ceramic materials: silicon nitride si₃n₄, 90%；Ytterbium oxide y₂o₃, 1-3%；Aluminium oxide al₂o₃, 0.5-1.5%；Oxidation Magnesium mgo, 0.2-0.5%；Lanthanum sesquioxide la₂o₃, 0.5-1%；Hafnium oxide hfo₂, 0.2-0.5%, aluminium nitride aln, 0.5-2%.

3rd, welding ceramics material: titanium carbide tic, 72%；Silicon nitride si₃n₄, 20-30%；Whisker carborundum sic, 0.2- 0.5%；Molybdenum silicide mosi₂, 0.1-0.2%；Aluminium oxide al₂o₃, 5-10%；Silicon oxide sio₂, 0.1-0.2%.

Remaining process conditions is identical with embodiment 1.

Claims

1. high-power silicon nitride ceramics heating plate, with silicon nitride as main raw material(s) it is characterised in that include insulated ceramic plates, Heating ceramic, welding ceramics and external wire, on the median plane of insulated ceramic plates, sintering has the conductivity ceramics of u shape arrangement, leads The two ends of electroceramics are connected with welding ceramics, and welding ceramics have one side to expose in insulated ceramic plates, are solder side, in solder side On be welded with external wire.

2. high-power silicon nitride ceramics heating plate according to claim 1 is it is characterised in that heating ceramic, by conductive Metal dust and nonconducting non-metal powder mix, and reach tune by the ratio adjusting metal dust and non-metal powder The effect of economize on electricity resistance, electrified regulation, reach the heating power of design.

3. high-power silicon nitride ceramics heating plate according to claim 1, it is characterised in that insulated ceramic plates, is thermal capacitance Measure big insulated compound pottery, intensity height, heat shock resistance, heat stability are high.

4. high-power silicon nitride ceramics heating plate according to claim 1 is it is characterised in that welding ceramics, fast electric energy Speed is conducted to heating ceramic, and itself does not generate heat thus protecting leading-out terminal temperature not high, safe wiring.

5. high-power silicon nitride ceramics heating plate according to claim 1 is it is characterised in that external wire, by metal wire It is welded in the exposed surface of welding ceramics it is ensured that outlet is firm, reliable.

6. high-power silicon nitride ceramics heating plate according to claim 1 it is characterised in that insulating ceramic materials by weight Ratio is as follows: silicon nitride si₃n₄, 91.5-94%；Ytterbium oxide y₂o₃, 1-3%；Aluminium oxide al₂o₃, 0.5-1.5%；Magnesium oxide Mgo, 0.2-0.5%；Lanthanum sesquioxide la₂o₃, 0.5-1%；Hafnium oxide hfo₂, 0.2-0.5%, aluminium nitride aln, 0.5-2%, all Composition weight is 100%.

7. high-power silicon nitride ceramics heating plate according to claim 1 it is characterised in that heating ceramic material by weight Ratio is as follows: silicon nitride si₃n₄, 40-50%, the solid solution of titanium carbide and titanium nitride, ti(c, n), 26-35%；Carbon in solid solution Change the weight of titanium and titanium nitride ratio for 4:6；Molybdenum powder mo, 0.5-3%；Nano nickel ni, 0.5-1.0%；Niobium carbide chnb, 0.2%；Brilliant Must carborundum sic, 0.2-0.5%；Molybdenum silicide mosi₂, 0.1-0.2%；Silicon oxide sio₂, 0.1-0.2%；Aluminium oxide al₂o₃, 5- 10%, whole composition weight are 100%.

8. high-power silicon nitride ceramics heating plate according to claim 1 it is characterised in that welding ceramics material by weight Ratio is as follows: titanium carbide tic, 60-72%；Silicon nitride si₃n₄, 20-30%；Whisker carborundum sic, 0.2-0.5%；Molybdenum silicide mosi₂, 0.1-0.2%；Aluminium oxide al₂o₃, 5-10%；Silicon oxide sio₂, 0.1-0.2%, whole composition weight are 100%.

9. the manufacture method of high-power silicon nitride ceramics heating plate hard outside soft inside is it is characterised in that step is as follows:

4th, overall hardening degumming；

5th, put into hot isostatic pressure stove hip stove to sinter, reinforcement, stiffened molding, 1800 DEG C -1820 DEG C of maximum sintering temperature, Pressure: 1500mpa；This Compound Machining forming process is commonly called as hard outside soft inside technique.