CN1066952A - The manufacture method of semi-conductor heating parts - Google Patents
The manufacture method of semi-conductor heating parts Download PDFInfo
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- CN1066952A CN1066952A CN 92101500 CN92101500A CN1066952A CN 1066952 A CN1066952 A CN 1066952A CN 92101500 CN92101500 CN 92101500 CN 92101500 A CN92101500 A CN 92101500A CN 1066952 A CN1066952 A CN 1066952A
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Abstract
A kind of manufacture method of semi-conductor heating parts.With the halide of tin, magnesium, titanium, iron, antimony, chromium, boron and tetraethoxysilane, ceruse, ammonium fluoride is the saturated solution that raw material is mixed with, atomizing diffusion in high temperature furnace, it is deposited on the good heatproof insulating body of purification becomes the surface radiation layer, after aging, coating insulation and installation lead-in wire form.Semi-conductive surface radiation layer has good light transmission, chemistry and thermal stability, and the electric heating transition effects is all arranged under the AC and DC electric field, can use for a long time below 800 ℃.
Description
The invention belongs to the semiconductor heat source technology, particularly about a kind of manufacture method of semi-conductor heating parts.
Along with the fast development of semi-conductor industry and electroheat technology, the turn up of electrothermal film technology especially, its electrothermal part adstante febre flames of anger, safe in utilization, thermal inertia is urinated in thermostatic control, electric conversion efficiency height, thereby obtains extensive use.As the PTC(electric ceramic) be with heat proof material mixed-formings such as the compound (as sodium sulphate, barium titanate etc.) of some element and porcelain powder, roasting forms in kiln, its conductive characteristic is a positive temperature coefficient, resistance raises with temperature and increases, uprush when reaching Curie temperature and reach temperature control, using below 300 ℃.And for example the DZR(electronically electric heat is handled), be to adopt electric conducting material to add inorganic or organic film forming agent to be sprayed on indirectly on the surface of high-temperature insulation body, form the microcosmos network conductive coating through sintering.CN1034107A(application number 88100015.9) the DZR technology that provides is to use Sncl
45H
2O is dissolved in the organic solvent, adds reducing agent (Sbcl
3, NH
4F, CF
2COOF etc. choose any one kind of them) it is free in 350～550 ℃ of high temperature airs decompose and be reduced into the semi-conductive divalence of this kind, univalent oxide and molecule mixture (routine SnO
2+ SnO+Sn) plating is advanced the high-temperature insulation body and is formed, also propose on the patent to make the large power, electrically heat exchange body with the way of stack.PTC shows as whole charged after energising, can not make container on-line equipment liquid heat; And present DZR technological processing craft comparatively falls behind, the reliable and consistency of finished product is relatively poor, can not keep high-transmittance, and serviceability temperature is subjected to limit (below 300 ℃).
The objective of the invention is to select for use and can form the semi-conductive element of hyperthermia radiation and compound thereof and adopt new technologies such as electric jet, atomizing diffusion, ion sputtering to prepare large-area radiating layer, its heat efficiency height, transparency height, and can use above under 300 ℃ the temperature.
The present invention is according to the lattice defect theory, the strict energy gap of selecting semiconductor element, adjust the additional energy of atom, under certain thermal field condition, make it shape in interatomic ionic bond and covalent bonds, make the ordering of radiating layer lattice then, can obtain all good semiconductor high temperature face radiating layer of chemical stability and thermal stability.
The semi-conductor heating parts manufacturing process is divided into matrix purification, diffuse source preparation, spreads to mix and handle and four steps of reprocessing as shown in drawings:
(1) matrix purifies.Matrix can be heatproof insulating materials such as glass, enamel, pottery, temperature resistant rubber, heatproof plastics, various laminated material and mica, quartz.Glass, enamel, pottery are earlier with washing agent and clean water flush away surface contaminants, clean with deionized water again, in case of necessity need be with 5% HF or 10～20%KOH(or NaOH) solution-treated, use deionized water and absolute ethyl alcohol double purification then, carry out drying after being neutrality.Temperature resistant rubber, heatproof plastics and lamination heatproof insulating material adopt the udst separation method to handle.Purification is preferably under the ultra-clean condition and operates.
(2) diffuse source preparation.The prescription of the raw material variety that uses is:
Tin halides (SnXn, X=cl, Br; N=2,4) 60.0～99.0%
Magnesium halide (MgX
2, X=cl, Br) 0.0～2.0%
Halogenated titanium (TiXn, X=cl, Br; N=2,4) 0.0～2.0%
Ferrous halide (FeX
2, X=cl, Br) 0.0～2.0%
Antimony halides (SbXn X=cl, Br; N=3,4) 0.0～2.0%
Tetraethoxysilane (C
2H
5O)
4Si 0.0～30.0%
Halogenation boron (BX
3, X=cl, Br) 0.0～2.0%
Hafnium halide (CrX
3, X=cl, Br) 0.0～2.0%
Ceruse (PbCO
3) 0.0～10.0%
Ammonium fluoride (NH
4F) 0.0～10.0%
With 40～70% absolute ethyl alcohol, the complexity control of looking its dissolving adds the hydrochloric acid of 30% concentration during preparation, and the hydrofluoric acid of 30～45% concentration adds a spot of chloroazotic acid in case of necessity.
(3) processing is mixed in diffusion.Place the diffusing, doping kiln with purifying the good first-class clamping apparatus of matrix, heat up in the uniform temperature district (300～800 ℃) make its uniform deposition on the surface of matrix the diffusion that fully atomizes of its diffuse source.Preferably in the airtight vacuum high temperature furnace, carry out the ultra-clean atomizing and handle, can obtain the even high temperature face radiating layer of high-transmittance.Base shape, material difference during processing, its diffuse source, treatment temperature, processing time and pressure are all different.The diffusion time of mixing is 10min～3h., and thickness is 5～50 μ m.The matrix of handling well is called the semiconductor hot body.For the glass transparent matrix, in order to keep its transparency and reliability, should carry out ion sputtering earlier, form good substrate, spread again.The radiating layer of making like this is even, and firmly, hot ability to bear increases.
By adjusting input variable, raw material proportioning, furnace temperature and the diffusing, doping time of diffuse source, can obtain the radiating surface required value of different-thickness, different surfaces resistance, different capacity and different serviceability temperatures.The face resistance mean value error of surface radiation layer is below 10%.
(4) reprocessing.Semi-conductor heating parts is carried out the aging and heat ageing of electricity, its objective is the lattice ordering that makes the semiconductor surface radiating layer and improve thermal stability.Electricity is aging to be it to be divided into 4～5 retainings carry out electricity and wear out below operating voltage, and ageing time is 10～30min under every retaining voltage; Heat ageing is that semi-conductor heating parts is placed high temperature furnace, is divided into 3～4 retainings to the rated temperature in room temperature and carries out heat ageing and handle, and every retaining ageing time is 4～8h..Aging good semi-conductor heating parts is coated with insulation and makes it to finish the semi-conductor heating parts moulding with installation telegram lead-in wire (promptly adopting general electric heating appliance lead-in wire method to be connected the input and output line).
With the semi-conductor heating parts that the present invention makes, under the energising heating state, water on the spray, strong acid, liquid do not influence use after the link electrode place takes seal protection layer, even put it into still operation as usual in the water.To put into oil under 150 ℃ missing of ignition being lower than; Can toast down moist gunpowder, explosive and fool proof with it being lower than 150 ℃.Make that to pull the shape heating glass transparent, use in winter and can not play steam.The temperature that semi-conductor heating parts uses is decided on the heat-resisting degree of base material, can use down at 800 ℃ as the semi-conductor heating parts of making on quartz glass; Use even more ideal on the devitrified glass.Be quite long the useful life of this semi-conductor heating parts, as with mica and pottery be the warmware of matrix respectively at 300 ℃, can use continuously under 500 ℃ and not see variation more than thousands of hours; If low temperature (as 120～130 ℃) slightly down use can reach up to ten thousand hours and also not see to some extent and change.
The present invention compared with prior art its characteristics is: (1) will mix on the high temperature insulation medium spreading under the thermal field condition through the compound of the chemical element of screening, and forming uniform high temperature face radiating layer, this diffuse source is infiltrated in the lattice of dielectric and is become very firm chemical bonding structure.
(2) manufacturing process of semi-conductor heating parts has adopted semiconductor diffusion principle and process, especially the strict energy gap of selecting semiconductor element, with the new ideas of adjusting discontinuous additional energy, under certain thermal field condition, form interatomic ionic bond and covalent bonds, and make its lattice ordering.
(3) the surface radiation layer of semi-conductor heating parts has good chemical stability and thermal stability; Except in certain warm area, under external interchange of the flames of anger or the DC electric field electric heating transition effects being arranged all; Has capacitance characteristic significantly; Corrosion resistance, light transmission and quite long useful life thereof are preferably arranged simultaneously.
Example one
After 275 * 100mm dark-brown glass usefulness ethanol purified treatment drying, on its working face, spray the ethanolic solution of the tetraethoxysilane of the about 0.05mm thickness of one deck, and under 200 ℃, be cured.Again with 90.0% Sncl
4, 5.0%Bcl
3, 1.0%Sbcl
5Use 60% absolute ethyl alcohol respectively, the mixed solvent that 39.5% hydrochloric acid (containing Hcl30%) and 0.5% hydrofluoric acid (containing HF30%) are formed is dissolved into saturated solution; And PbCO
3Then in above-mentioned mixed solvent, add a small amount of chloroazotic acid and make it be dissolved into saturated solution, it is mixed into diffuse source.The glass of handling well pulled insert in the diffusion furnace, clip anchor clamps, be warming up to 450 ℃ and maintenance, under this temperature, diffuse source atomized to handle and import in the stove, mix processing procedure through finishing diffusion behind 10～20min, can make the high light transmittance semi-conductor heating parts, through after electricity and the heat ageing, wiring heating glass.
Example two
The high alumina ceramic of 300 * a 200 * 6mm is pulled, and the KOH solution with 10% soaks 15min, purifies with deionized water again, and the matrix working face is neutral after the dried.Carry out double purification, dried through absolute ethyl alcohol again, clip clamping apparatus at its matrix working face, the about 0.2mm tetraethoxysilane of spraying one deck places diffusion furnace to be cured under 200～400 ℃ of temperature on working face.Again with 92.0%Sncl
4, 2.0%Ticl
4, 2.0%Sbcl
5, 1.0%PbCO
3, 2.0%Mgcl
2, 1.0%Fecl
3Be mixed with saturated solution with mixed solvent, constitute diffuse source.The diffuse source back that fully atomizes is imported in the diffusion furnace, and Control for Kiln Temperature feeds nitrogen and mixes process with protection at 450～550 ℃, finishes through 15～25min process.Promptly obtain semi-conductor heating parts.
Claims (7)
1, a kind of manufacture method of semi-conductor heating parts, it is characterized by with the halide of tin, magnesium, titanium, iron, antimony, chromium, boron and tetraethoxysilane, ceruse, ammonium fluoride is the solution (being referred to as diffuse source) that raw material is made into, making its atomizing be diffused in temperature is in 300～800 ℃ the high temperature furnace, be deposited on through on the heatproof insulating body of purified treatment, its time is 10min to 3h, then under working voltage and serviceability temperature, carry out the aging and heat ageing of electricity, be coated with insulation then and finish with lead-in wire is installed.
2, the method for claim 1 is characterized by the raw materials used proportioning of diffuse source and is:
Tin halides (SnXn, X=cl, Br; N=2,4) 60.0～99.0%
Magnesium halide (MgX
2, X=cl, Br) 0.0～2.0%
Halogenated titanium (TiXn, X=cl, Br; N=2,4) 0.0～2.0%
Ferrous halide (FeX
2, X=cl, Br) 0.0～2.0%
Antimony halides (SbXn X=cl, Br; N=3,4) 0.0～2.0%
Tetraethoxysilane (C
2H
5O)
4Si 0.0～30.0%
Halogenation boron (BX
3, X=cl, Br) 0.0～2.0%
Hafnium halide (CrX
3, X=cl, Br) 0.0～2.0%
Ceruse PbCO
30.0～10.0%
Ammonium fluoride NH
4F 0.0～10.0%
With ethanol, hydrochloric acid, hydrofluoric acid, nitric acid are with the raw material dissolving and be mixed with saturated solution.
3, method as claimed in claim 2, it is characterized by ethanol is absolute ethyl alcohol, use amount is 40～70%; Look its dissolving difficulty or ease and add the hydrochloric acid of 30% concentration, 30～45% hydrofluoric acid, add a spot of chloroazotic acid in case of necessity to dissolve it.
4, the method for claim 1, it is characterized by described matrix is glass, pottery, enamel, heat resistant rubber, plastics, laminated material, and mica, quartz etc.; Purified treatment be in common washing back with deionized water, absolute ethyl alcohol, NaOH or potassium hydroxide solution and hydrofluoric acid treatment it.
5, the method for claim 1, it is characterized by described electricity aging is to be divided into 4～5 retainings in working voltage and following scope thereof, aging 10～30min under every retaining voltage; Described heat ageing is meant at normal temperature and is divided into 3～4 retainings to the serviceability temperature scope, aging 4～8h. under every retaining temperature.
6, the method for claim 1 is characterized by described matrix purification and carries out under the ultra-clean condition.
7, the method for claim 1 is characterized by described atomizing diffusion process and carries out under vacuum tightness.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92101500 CN1024978C (en) | 1992-03-07 | 1992-03-07 | Method for manufacturing semiconductor heating element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92101500 CN1024978C (en) | 1992-03-07 | 1992-03-07 | Method for manufacturing semiconductor heating element |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1066952A true CN1066952A (en) | 1992-12-09 |
| CN1024978C CN1024978C (en) | 1994-06-08 |
Family
ID=4939152
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92101500 Expired - Fee Related CN1024978C (en) | 1992-03-07 | 1992-03-07 | Method for manufacturing semiconductor heating element |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1024978C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1314828C (en) * | 2004-11-23 | 2007-05-09 | 江苏工业学院 | Method and apparatus for DC electric field accelerating solid powder boriding |
| CN100349498C (en) * | 2003-10-17 | 2007-11-14 | 杨金林 | Electric-heating film and manufacturing method thereof |
-
1992
- 1992-03-07 CN CN 92101500 patent/CN1024978C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100349498C (en) * | 2003-10-17 | 2007-11-14 | 杨金林 | Electric-heating film and manufacturing method thereof |
| CN1314828C (en) * | 2004-11-23 | 2007-05-09 | 江苏工业学院 | Method and apparatus for DC electric field accelerating solid powder boriding |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1024978C (en) | 1994-06-08 |
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