DE1583477A1 - Heat treatment process - Google Patents

Description

PHB »

-.Pipl.-lng. ERiCM E. WALTHER
Registration: fU _P PHiLIPS '

e ;: PHB-31.666
Registration dated Aug. 22, 1967

Heat treatment process.

The invention relates to a method lungs' Wärmebehand- ■.

When a mass of material is in a den If steam from a furnace containing a substance under bruok is subjected to a heat treatment, visually

occur oa, the pressure may rise so äohnell, k ί the furnace bursts.

The invention is based on the knowledge that the steam druol: in a large room through the Κ # 1 deadline I,. Hauuas will join.

- 2 "- 1 EP '.} / 77 PHB.31666 After Ürfindun ^ ¹ a process is carried out at aur ■"' ■ ^ Waruebohandlun a furnace containing the Ofenrauia i leaving a material in a battle stohenien a pressurized ^substance! A pipe with a liquid plug of the substance connected to a pressure source and the Ueizuii;:; is

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in such a way that the part of the furnace space adjoining the plug is the coldest part of the furnace space and the? Tenporature along the pipe a inlet in the direction away. from the adjoining the plug part of the oven compartment, thereby at Druehanstieft in Of enrauw the Flitssigkeit / vapor interface of the substance naoh a colder part of the tube and drop in pressure in the furnace chamber NaOH m hotter part dos tube "moves the erfiudungsgemässe. Method can easily be self-regulating machon with respect to the arbitrary temperature and Druakschwankunijen that normally-occur without the provision of a working with a τ ehr high Sicherheit.igrad Temporaturreselvorrichtunc ^1, · "■

The mass of the ratorials can be crushed in porm or in the form of a solid, '"bodya, for example in Binkristall ·» form. to be present. According to the Behaiiä ^ unij the material can be in shredded For! " or i if Q3 selects the treatment total "

's - · ■

zen is, in Ρϋϊ · ;; τ eitien solid body remain. If a crystal germ is needed, e "iu ^ ahfaii ^ o zöricloinerte mass

ÖIN initially polykriatailiner firmer. ^ örpei naoh the Sohmeifift ■ '

in a single-room förüf «rsturreni; / "■ -

It can be beneficial | -if a pertaining to the liquid Subatitna inorteo gas pressure on the grafting »ü8Ü1lt | and on thsSt "farther voiii Ofenräujn IHnfjlr the pipes lying * Söitt

. ■ I
dea Pf'ropfiSiiiB works «

009834/0262

The plug can be in a toilet of the pipe with a Bore to be arranged · This part n with a length Bohrun.j bow acts on dampening · the movement of the plug » • what can ■ be desirable if it is possible that a hawser

Fluctuations in the conditions in the furnace chamber "and this damping can also contribute to maintaining the specified partial gradient length of the tube * so that the heat flow along the tube and through the plug removed from the furnace chamber is limited to a certain value." The heat treatment can be a zone of melted sheet metal, whereby the steam is absorbed into the material. The material can be germanium, initially either intrinsic or polluting, and the substance can be "mercury " - ^; .- * ■ - ■■ - ..
".. '■ ._ ■ --- ■■ ,, Basι firfiitdungsgeniasne process has ALSs a befriedi ^ artde alternative of in J» App.-rhyB.Vol "33 * Mo _t10 October» 19621 Seiteil -. 294T to 2950, in which "it haiset that Gernanium was obtained in a concentration of 8 Sj 10 ■ and 5 ac 10 tiuecksilberatomen / cni in an Openeneri ^ SySteffi and not under pressure. Froa" H & tios | al iJlectrüiiiiss Conferonoö VoI * ly (1963) Papar 1656 pages 635 Ms : ': $ ίί Beaohreibt a method by means of

its aural consistency from 0.5 χ 10 'to 1 χ 10 * Queckeilixerafiöirißn / om has been obtained, with only obtaining the pressure required to maintain a higher Offer what / iahohmal «rwünacht is, a zuiöhmoleene Ämpull «Verwehd, * t: Wii» Ä »■".-.-

0098 3 4/02 62 bad ordinal

The furnace can only perform zone wax heat treatment generally be heated with the aid of a first system ^ and to melt a zone of the material, a zone can be used Heating by a second heating system in relation to the furnace space moved will * be causedβ

For germanium and mercury, the furnace can do this are heated that in the permanent state di® low temperature

in the furnace chamber there is swisohen 45O ⁰ C and 500 ⁰ C «It was fixed» ■ "■■■■■ - .. ■ '■ - ■« *

represents that with a lowest temperature of 480 ^Q C in the furnace chamber a doping level for germanium of 2 χ 10 Queoksilberatomen / om is achievable.

The invention also relates to a mass of according to a method according to the first aspect of FIG Invention of a material subjected to heat treatment »

An embodiment of the inventive method the following is described as an example »whereby the ti ·! - liögend.haematic drawing is referenced, which is a «pre ^ riohtung sseig.t »

The figure shows a semicircular crucible 1 made of high-purity Kieöelerdehyde, which contains polycrystalline germanium 2 and a crystal nucleus 3. ".- ■ '..' ■ '

The crucible 1 is arranged in an elongated tube 4 * of silica, one end 5 of which is melted and the other end of which is connected to a tube 7 of a small office space which contains a part 8 with a narrow bore. Tell B. is coiled and can be a length of oa, 1 foot ». along the Röhra ^ eaieasen, and a bureau knife from ^ - to 1 putty. * The iiohr 7 contains a container 9 with a Queok-

0 0 9 8 3 4/02 5 2 '■' ... bad original-

- 5 "" PHB.51666

silver plug 10.

Dao tube 4 -is inclined downwards in the direction of the 3 end 6 an-I has an inner y / and 11, against which a small buyer igt broken kioselelerdo 12

The furnace axi ·;!, That is the space within the pipe · 4 and the space connected with it in the pipe f up to the (Jueokeilber 10, is generally heated with the help of a first shark system - ge «·, daa as one There is a resistance heating part wound around the ear 4 and two cattle parts 14, which provide for a correction at the ends so that the furnace is heated essentially uniformly, but the end adjacent to the mercury 10 is the coldest part of the furnace chamber »

For Local heating zone for melting of the 'germanium 2 provides a second heating system, which is verBohiebar and aug a Wideratandeheisstöil 15 bsstoht, ti v a can pein a zylinderföraigen liohli'.örper arranged Swirl. "

In the followandeti the sequence of actions becomes beaohriebgn «

If the end 5 of the tube 4 is still open, will the heap 12 made of silica and the one with dom germanium 2 and The crucible 1 provided with the seed 3 is arranged in the tube 4 The end * 5 dee Hohya 4 is then partially closed, this for the Relief; of the later addition: ir.enechEi0lzons "

Bas knee 6 äen-Bohrs 4 is made with the Rohy 7 v *? Ljun4fll | because "-'kintßv the BefeÄlttsc 9 rait tin" m verzweiipten tubular T * ^ - blndung ■ stands desaen a © j? Arm 18 by means of one tap 19 4 ^ * a (not shown) i »an evacuation system -vt ^ · d yarvakuumpUMpe, and deatsen other A? M 20 mlttila a ·· ι

Hahns 21 with a Qjielle (not shown) under pressure standing nitrogen is connected * A pressure gauge 22 is arranged on the branched pipe between the taps 19 and 21.

A hole is made in the Hohr 4 at 16, the Mercury was put in the tube through the hole at 16 "wonai ^ h the hole is closed again, J) aa mercury is behind the wall 11 is held in the low lilnda of the ear 4.

The end 5 of the ßohrs'4 is with a diffuser pump connected »which is in the Evakttiörungssytem, which contains the backing pump connected to the arm 18 '' Das Tube 4 is used up to a Üruok of, for example, 2 / um mercury silbersäuie evacuated »and the end 5 is closed.

The end parts 14 as well as the sliding part 15 are set in their position and the heating systems are switched on in order to increase the temperature of the furnace room in general to about 6O ⁰ G and to form a zone of molten germanium adjoining the crystal nucleus 3,

The cock 19 is closed and by regulating the cock gl, Bruqk ypn dü3? Stickatoffqutlle introduced, $ a should be noted that the formation of qints druoka by evaporation of the mercury must be stored for 10, 2 years.

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Since β G er manu im 2 becomes t | * naol * by shifting of Teila 13 zonu'nweise the V / ärr.ie ',' * u8gtSQi; Bt, · and from hi «r verich, iffe # aioh the zone nuoh the link # ii seltt the? i§utt The re-solidified germanium is a single crystalline substance, 4ft duroh 4 · η germ 3 krigtaUiöiert and with mercury also the. , surrounding (mercury containing AtnioephÄPe is endowed "

15834 ?? ⁰ · ³¹⁶⁶⁶ ·

Is Dar valve 21 is closed and the valve 19 partially open, so that the nitrogen slowly through the VoryaUuumpuiiipe sucked "Finally the tap is fully opened l'J and from that moment on, the mercury is sucked back into the container 9 10th

The heating system © is switched off and the germanium 2 can cool down. The cock 21 is closed, the The end of the eolir 4 is opened and the crucible 1 is removed from the tube

During the 2-zone heating, an accidental fluctuation can cause the Dtuok to rise in the furnace chamber. "This can be seen from the fact that the mercury 10 is pushed away from the end 6" and the pressure of the mercury vapor drops as the mercury IQ is removed from the furnace chamber a'; cold atm to add part of the pipe 7 »

The opposite effect occurs through a accidental lowering of the pressure in the furnace chamber * The arrangement of the Part 8 takes care of a movement that is too fast of the mercury 10 and also forms a means of observation of the Temperaturgiflillee along the Hohr 7

With the selected pressure equilibrium, which is determined by the height of the mercury 10 and the pressure resulting from the nitrogen source, mercury dissolves in the glass until the state is reached in which the vapor pressure over the solution corresponds to the pressure supplied so that the Queol.oiiber in the treated germanium mnd just · if the Seigerungagrad of ciueoksilbera in Germariium of iangewandten DruokabhSngig "is a case durohsohnittliobiin _(temperature in the furnace room of about 6O0 ° c can you genaoht minimum temperature in Ofönraum easily awiaohen 45O ⁰ C and 50O ⁰ G will,

00983470252 BAD oriqinal

Claims (2)

PΑΐΚίίΤΑϊ; S PHÜ UHui t ~ 1. Process for the heat treatment of a "4asse one Material in a furnace containing the vapor of a pressurized substance, characterized in that Furnace space by means of a pipe with a; liquid plug of the Substance connected to a pressure source and the heater in such a way is? that the on. the "part bordering the plug" the coldest part of the stove. and the temperature is longitudinal of the pipe from the Φβΐΐ of the furnace adjacent to the plug in a direction away from this furnace space decreases, whereby the liquid / l) ar: ipf Grenzf lache be ± pressure rise in the furnace space the substance after a colder feil dee tube and in the event of a pressure drop iti; Oven space moved to a hotter part of the pipe. - 2. The method according to claim 1, characterized in that that by means of a gas which is inert with respect to the liquid substance, pressure is exerted on the plug, which on the further from the Ofeniauffl along the deaHohrs lying® side of the plug acts »- '; 3 · Method according to claim 1 or 2, characterized in · » draws that the plug is in one part of the pipe with iiner engin bore arranged iat, 4. Method according to one of the preceding claims, characterized in that the Wärraebishandliing is a gonen Bohmelz treatment is, with the Dfimpf in the material * ufgenoneien will, 5 »Method ^ naoh one of the preceding claims»; daduroh marked »that the» material Öerroftnium and the Subat & ne mercury is » 00 98 3 4 / 02S2. bath Method according to claim 4 or 5, characterized in that the furnace is generally heated by means of a first heating system, and local heating is brought about by a second heating system which is moved in relation to the furnace to melt a zone of the material is · 7 · the method of claim (and 5 or 6, daduroh 'ej-ekeiinaeichnet "that the Ofenraun .If heated such that in the steady state, the lowest temperature I'm Ofenraura between 45O ⁰ C and 5QO ⁰ C. L e r s e i t e