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公开(公告)号：US5383982A
公开(公告)日：1995-01-24
申请号：US166254
申请日：1993-12-13
CPC分类号： C23C22/10
摘要： A process of producing a phosphate coating on a metal surface of iron or steel by contacting the surface with an aqueous phosphating solution on the basis of magnesium phosphate. The solution contains 0.2 to 4 g/l magnesium, 1 to 20 g/l phosphate (calculated as P.sub.2 O.sub.5) and a peroxide compound as an accelerator. The phosphating solution is free of inorganic substances which are not precipitable with calcium hydroxide in a neutral or alkaline medium. It is preferred to use phosphating solutions which also contain activators, which are precipitable with calcium hydroxide in a neutral or alkaline medium.
摘要翻译： 一种通过使表面与磷酸钙水溶液接触而在铁或钢的金属表面上生产磷酸盐涂层的方法。 该溶液含有0.2至4g / l的镁，1至20g / l磷酸盐（以P2O5计）和过氧化物作为促进剂。 磷酸盐溶液不含在中性或碱性介质中不能用氢氧化钙沉淀的无机物质。 优选使用也含有活化剂的磷酸盐溶液，其可以在中性或碱性介质中用氢氧化钙沉淀。
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公开(公告)号：US5165795A
公开(公告)日：1992-11-24
申请号：US727427
申请日：1991-07-09
申请人： Dieter Hauffe
发明人： Dieter Hauffe
CPC分类号： G01G9/00 , G01N21/8422 , G01J5/52 , G01N2021/8427
摘要： A method of determining the weight per unit of area of conversion layers, particularly of phosphate layers, on metals, in which the heat radiated from the dry surface which is covered with the conversion layer and is at the temperature T and the heat radiated from a reference surface or a reference cavity which is at the temperature T+t are periodically measured at a temperature between 15.degree. and 50.degree. C. by a wavelength-insensitive electic infrared detector. t is preferably selected in the range from +15.degree. to +3.degree. C. from -15.degree. to -3.degree. C. above or below T. The weight of the conversion layer per unit of area is determined from the amplitude of the resulting electric alternating signal. The radiant heat is suitable measured by an infrared detector having a sensor which consists of a pyroelectric sheet of polyvinylidene fluoride.
摘要翻译： 确定金属上转化层，特别是磷酸盐层的每单位面积的重量的方法，其中从被转化层覆盖并处于温度T的干燥表面辐射的热量和从其中辐射的热量 在温度为T + t的参考表面或参考空腔中，通过波长不敏感的电红外探测器在15°和50°C的温度下周期性地测量。 t优选在-15℃至-3℃的范围内在+ 15℃至+ 3℃的范围内选择，高于或低于T。每单位面积的转化层的重量由所得到的振幅 电交流信号。 辐射热适用于由具有由聚偏二氟乙烯的热电片组成的传感器的红外检测器测量。
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公开(公告)号：US5039361A
公开(公告)日：1991-08-13
申请号：US443212
申请日：1989-11-28
申请人： Dieter Hauffe , Jorg Hieke , Rudolf Vey , Gunter Siemund , Han-Yong Oei
发明人： Dieter Hauffe , Jorg Hieke , Rudolf Vey , Gunter Siemund , Han-Yong Oei
摘要： During a method of phosphating a metal surface which includes at least in part iron or steel and is dipped into or flooded with a phosphating solution which contains layer-forming cations and nitrate or equivalent accelerators, the iron content is limited by a precipitation of iron phosphate. A partial volume of the phosphating solution is intermittently withdrawn from the bath tank and in a separate aerator is contacted with oxygen or an oxygen-containing gas. The iron phosphate sludge is removed from the resulting solution, which is then returned to the bath tank. The partial volume of the phosphating solution is supplied from below into and is aerated in an aerator, which is provided with an aspirating aerating agitator and which is tapered at least in its lower portion. When the aerator has been terminated, the phosphating solution which has been depleted of iron(II) is sucked off upwardly and is returned to the bath tank.
摘要翻译： 在磷化金属表面的方法中，该金属表面至少部分包括铁或钢，并浸入含有形成层的阳离子和硝酸盐或等效促进剂的磷酸盐溶液或淹没物中，铁含量受磷酸铁沉淀的限制 。 将部分体积的磷酸盐溶液间歇地从浴槽中取出，并且在单独的曝气器中与氧气或含氧气体接触。 从所得溶液中除去磷酸铁污泥，然后将其返回到浴槽。 磷酸盐溶液的部分体积从下方供给到曝气器中，曝气器设置有吸气式充气搅拌器，至少在其下部逐渐变细。 当曝气器已经被终止时，已经耗尽铁（II）的磷化溶液被向上抽吸并返回到浴槽。
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公开(公告)号：US4867853A
公开(公告)日：1989-09-19
申请号：US106165
申请日：1987-10-07
摘要： Disclosed is a process of producing a phosphate coating on a composite part consisting of steel and galvanized steel, which comprises alkaline cleaning, rinsing with an aqueous rinsing bath, and phosphatizing with an aqueous zinc phosphate solution. The formation of a non-uniform coating and of spots is avoided in the process of the invention by the use of a rinsing bath which contains at least 0.2 g/l alkali borate, at least 0.1 g/l alkali silicate and at least 0.05 g/l alkali nitrite, and which preferably contains said components in a total up to 5 g/l.If the composite part is to be activated with an activating bath which contains titanium phosphate before being contacted with the zinc phosphate solution, the activating bath must contain at least 1 g/l and preferably up to 4 g/l of tetraalkalipyrophosphate.The process of the invention can be used to prepare composite parts of steel and galvanized steel for subsequent painting, particularly by electrophoretic dip painting.
摘要翻译： 公开了一种在由钢和镀锌钢构成的复合部件上生产磷酸盐涂层的方法，其包括碱性清洁，用水性漂洗浴漂洗，并用磷酸锌水溶液磷酸化。 在本发明的方法中，通过使用含有至少0.2g / l碱金属硼酸盐，至少0.1g / l碱性硅酸盐和至少0.05g / l碱式亚硝酸盐，并且其优选地含有总计高达5g / l的所述组分。 如果复合部件在与磷酸锌溶液接触之前用含有磷酸钛的活化浴活化，则活化浴必须含有至少1g / l，优选至多4g / l的四烷基磷酸盐。 本发明的方法可用于制备钢和镀锌钢复合材料，用于随后的涂漆，特别是通过电泳浸涂法。
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公开(公告)号：US4897128A
公开(公告)日：1990-01-30
申请号：US178183
申请日：1988-04-06
申请人： Heinz Dosch , Dieter Hauffe , Horst Gehmecker
发明人： Heinz Dosch , Dieter Hauffe , Horst Gehmecker
CPC分类号： C23C22/77 , G01N31/164
摘要： Described is a process for determining the zinc content of an acid aqueous phosphating bath. A bath sample is titrated at a pH value between 1.2 and 1.7 in the presence of ethylenediaminetetraacetic acid, hexamethylenetetramine and alkalihexacyanoferrate (III) with an alkalihexacyanoferrate(II) until the potential at an oxidation-reduction electrode immersed into the bath sample reaches an inflection point.Any content of nitrite and/or iron(II) ions must be removed by an addition of nitrite-destroying substances and by an oxidation to iron(III) ions at a pH value above 8.The process is particularly suitable for determining the zinc concentration of phosphating baths which contain 0.4 to 2.0 g/l Zn. The presence in phosphating baths of additional cations such as manganese and/or calcium and/or nickel and/or magnesium does not interfere with the process. The analysis can be automatic and may directly be used to control a metering device for supplying make-up concentrates to the phosphating bath.
摘要翻译： 描述了确定酸性磷酸氢盐浴的锌含量的方法。 在乙二胺四乙酸六亚甲基四胺和碱金属氰化铁酸盐（III）与碱金属氰化铁酸盐（II）的存在下，在1.2至1.7的pH值下滴定浴样品，直到浸入浴液样品中的氧化还原电极的电位达到拐点 。 亚硝酸根和/或铁（II）离子的任何含量必须通过加入亚硝酸盐破坏物质和通过氧化成铁（III）离子在pH值高于8处去除。该方法特别适用于测定锌浓度 的含有0.4〜2.0g / l Zn的磷化浴。 存在附加阳离子如锰和/或钙和/或镍和/或镁的磷化浴不会妨碍该方法。 分析可以是自动的，并且可以直接用于控制用于向磷化浴提供补充浓缩物的计量装置。
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公开(公告)号：US4597806A
公开(公告)日：1986-07-01
申请号：US751102
申请日：1985-07-02
申请人： Dieter Hauffe
发明人： Dieter Hauffe
CPC分类号： C23C22/77 , G01N31/164 , Y10T436/116664
摘要： In a process for maintaining a given zinc content in nickel-containing zinc phosphate baths,(a) nickel is precipitated in a bath sample by addition of dimethylglyoxime, a soluble copper complex compound is added and the liquid is then titrated against a copper-sensitive electrode, for determining the zinc content, with a volumetric solution containing a complexing agent for zinc and copper;(b) the automatic metering of zinc-containing supplementary concentrate is then regulated on the basis of the deviation, ascertained in this way, from the given zinc content (prescribed value).
摘要翻译： 在含镍磷酸锌浴中保持给定锌含量的方法中，（a）通过加入二甲基乙二肟将镍沉淀在浴样品中，加入可溶性铜络合物，然后滴定该液体以对铜敏感 用于测定锌含量的电极与含有锌和铜络合剂的体积溶液; （b）以含锌补充浓缩物的自动计量为基础，以此方式从给定的锌含量（规定值）确定偏差。
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公开(公告)号：US5294266A
公开(公告)日：1994-03-15
申请号：US978193
申请日：1992-11-18
申请人： Dieter Hauffe , Thomas Kolberg , Gerhard Muller , Horst Gehmecker , Werner Rausch , Peter Schubach , Thomas Wendel
发明人： Dieter Hauffe , Thomas Kolberg , Gerhard Muller , Horst Gehmecker , Werner Rausch , Peter Schubach , Thomas Wendel
CPC分类号： C23C22/73 , C23C22/34 , C23C22/361 , C23C22/60 , C23C22/83
摘要： The invention is in a composition and process for the chromium free passivating postrinsing of conversion layers on metals before the application of a paint or adhesive. The conversion layers can be on the bases of phosphate layers, at least two polyvalent metal ions with complex formers, titanium, zirconium and/or hafnium. The postrinsing agent is an aqueous solution which has been adjusted to a pH value of up to 5 and which contains an aluminum fluorozirconate having an Al:Zr:F mole ratio of (0.15 to 8.0):1:(5 to 52), and in which solutions the total concentration of Al+Zr+F is 0.1 to 8.0 g/l. The postrinsing solutions may additionally contain at least one of the anions benzoate, caprylate, ethyl hexoate, salicylate in a total concentration of 0.05 to 0.5 g/1 and may preferably be adjusted to the required pH value with cations of volatile bases, such as ammonium, ethanolammonium and di- and triethanolammonium. The paint is subsequently applied suitably by cathodic electrocoating or powder coating or from a low-solvent high-solids paint.The rinsing treatment is over a period of 1 to 120 seconds at temperatures of 20.degree. to 80.degree. C. The invention is used as a pretreatment to the application of a paint coating, film coating or adhesive coating.
摘要翻译： 本发明是用于在施加涂料或粘合剂之前的金属上的转化层的无铬钝化的组合物和方法。 转化层可以在磷酸盐层，至少两种具有复合成型剂的多价金属离子，钛，锆和/或铪的基础上。 postrinsing剂是一种水溶液，其pH值调至5以下，并含有Al：Zr：F摩尔比为（0.15〜8.0）：1：（5〜52）的氟锆酸铝， 其中Al + Zr + F的总浓度为0.1〜8.0g / l。 postrinsing溶液还可以含有至少一种阴离子苯甲酸酯，辛酸酯，己酸乙酯，水杨酸酯，总浓度为0.05至0.5g / l，并且可优选用挥发性碱如铵的阳离子调节至所需的pH值 ，乙醇铵和二乙醇胺和三乙醇铵。 随后通过阴极电涂或粉末涂料或低溶剂高固体涂料适当地施涂涂料。 在20〜80℃的温度下，漂洗处理时间为1〜120秒。本发明用作涂料涂料，薄膜包衣或粘合剂涂料的预处理。
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公开(公告)号：US4419199A
公开(公告)日：1983-12-06
申请号：US373475
申请日：1982-04-30
申请人： Dieter Hauffe , Gerhard Muller , Werner Rausch , Gudrun Volling
发明人： Dieter Hauffe , Gerhard Muller , Werner Rausch , Gudrun Volling
CPC分类号： C23C22/362 , C23C22/12
摘要： A process for the phosphatizing of metals, particularly iron, steel and zinc, in which the metal is contacted with acidic aqueous zinc phosphate solutions, containing an oxidizing agent, which containfrom 0.4 to 1.5 g/liter of Zn,from 0 to 1.3 g/liter of Ni andfrom 10 to 26 g/liter of P.sub.2 O.sub.5,and in which the weight ratio of Zn to P.sub.2 O.sub.5 is adjusted to a value of (from 0.012 to 0.12):1 and of Ni to Zn to a value of (from 0 to 1.5):1, and the bath is supplemented with a concentrate, in which Zn, Ni and P.sub.2 O.sub.5 are present in a weight ratio of (from 0.18 to 0.33:(from 0 to 0.06):1, so as to obtain satisfactory phosphatizing results over a long period.Preferably, the zinc phosphatizing solutions, which, in addition, may also contain simple or complex fluorides and compounds that reduce the weight of the coat, are applied at a temperature within the range of from 30.degree. to 65.degree. C.
摘要翻译： 一种金属，特别是铁，钢和锌的磷酸化方法，其中金属与酸性磷酸锌水溶液接触，含有氧化剂，其含有0.4-1.5g /升Zn，0-3.3g /升的Ni和10〜26g /升的P 2 O 5，并且其中将Zn与P 2 O 5的重量比调节至（0.012至0.12）：1，Ni至Zn的值（从 0至1.5）：1，浴中补充有以重量比（0.18-0.33：（0-0.06）：1）存在的Zn，Ni和P 2 O 5的浓缩物，以获得令人满意的 优选地，磷酸锌溶液还可以含有简单或复合的氟化物和降低涂层重量的化合物，其温度范围为30°至65° DEG C.
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公开(公告)号：US5203930A
公开(公告)日：1993-04-20
申请号：US570350
申请日：1990-08-21
申请人： Georg Blumlhuber , Horst Gehmecker , Dieter Hauffe , Lothar Kaul , Thomas Nitschke , Werner Rausch , Hardy Wietzoreck
发明人： Georg Blumlhuber , Horst Gehmecker , Dieter Hauffe , Lothar Kaul , Thomas Nitschke , Werner Rausch , Hardy Wietzoreck
CPC分类号： C23C22/184 , C23C22/13 , C23C22/22 , C23C22/362 , C23C22/73
摘要： A process for forming phosphate coatings on metal surfaces is provided which comprises the steps of contacting said metal surface with an Fe(II)-containing phosphating solution comprising0.4 to 30 g/l Zn4 to 30 g/l P.sub.2 O.sub.55 to 50 g/l NO.sub.3up to 10 g/l Fe(II) ; andup to 0.3 g/l (Fe(III)wherein the weight ratio of free P.sub.2 O.sub.5 to total P.sub.2 O.sub.5 is (0.04 to 0.50):1 and, replenishing said phosphating solution with Zn, NO.sub.3 and P.sub.2 O.sub.5 in a weight ratio ofZn:NO.sub. 3 P.sub.2 O.sub.5 =(0.60 to 0.30):(0.2 to 0.4):1.wherein the Fe(II) content is adjusted by oxidation with nitrate or nitrite derived from nitrate optionally employed with an oxygen-containing gas, H.sub.2 O.sub.2 and/or nitrous gases; and rinsing said metal surface with a cascade of at least two aqueous rinsing baths in the opposite direction of travel of said metal surface wherein water having a low salt content or no salt content derived from the phosphating bath is fed to the last rinsing bath and the overflowing water from said rinsing bath is fed to the next preceding rinsing bath and ultimately to the phosphating bath, and wherein the low salt content rinse water derived from the phosphating bath is withdrawn therefrom as a rate effective to permit the addition of phosphate-enriched rinsing water from the cascade of rinsing water to the phosphating bath while maintaining the desired species concentration in said phosphating bath.
摘要翻译： 提供一种在金属表面上形成磷酸盐涂层的方法，其包括以下步骤：使所述金属表面与含有0.4至30g / l Zn 4至30g / l P 2 O 5的含Fe（II）的磷酸盐溶液接触5至50g / l NO3高达10g / l Fe（II）; 和高达0.3g / l（Fe（III），其中游离P 2 O 5与总P 2 O 5的重量比为（0.04-0.50）：1，并用Zn，NO 3和P 2 O 5以Zn:Nn的重量比补充所述磷酸盐溶液 3 P 2 O 5 =（0.60〜0.30）：（0.2〜0.4）：1，其中Fe（II）含量通过硝酸盐或亚硝酸盐氧化而调节，硝酸盐或硝酸盐任选地与含氧气体，H 2 O 2和/或亚硝酸气体 并且在所述金属表面的相反行进方向上用级联的至少两个水性漂洗浴冲洗所述金属表面，其中具有低盐含量或不含有来自磷酸盐的盐含量的水被供给到最后的冲洗浴中， 将来自所述冲洗浴的溢出水进料到下一个先前的漂洗浴并最终送入磷化浴，并且其中从磷化浴中得到的低盐含量的漂洗水从其中提取出来，其速率可以有效地添加富含磷酸盐 从级联漂洗水 e向磷化浴中冲洗水，同时保持所述磷化浴中所需的物质浓度。
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公开(公告)号：US4849031A
公开(公告)日：1989-07-18
申请号：US92951
申请日：1987-09-04
申请人： Dieter Hauffe , Gisela Beege , Peter Mischke , Werner Rausch
发明人： Dieter Hauffe , Gisela Beege , Peter Mischke , Werner Rausch
CPC分类号： C23C22/362 , C23C22/77
摘要： Disclosed is a process of producing phosphate coatings on surfaces which consist of aluminum or its alloys and of at least one of the materials steel and galcanized steel by spraying or by spraying and dipping. Uniform phosphate layers having a high cover factor are obtained by the use of a phosphating solution which contains about 0.4 to about 0.8 g/l Zn, about 10 to about 20 g/l P.sub.2 O.sub.5, at least one accelerator and about 80 to about 220 mg/l fluoride ("F(el)"), as determined by a fluoride-sensitive electrode immersed into the bath solution and in which the content of free acid (FA) (in points) has been adjusted to and is maintained at a value corresponding to FA=(0.5 to 1.0)+K wherein K is calculated as K=(0.002 to 0.012).times.F(el). The free acid (FA) content is preferably adjusted to and maintained at FA=(0.04 to 0.06).times.C.sub.P.sbsb.2.sub.O.sbsb.5 +K and the content of free acid (FA) is determined using K=(0.003 to 0.009).times.F(el). The process is particularly suitable for preparing the surfaces for being painted, preferably by electrophoretic dip painting.
摘要翻译： 公开了一种通过喷涂或喷涂和浸渍在由铝或其合金和至少一种材料钢和镓化钢组成的表面上生产磷酸盐涂层的方法。 通过使用含有约0.4至约0.8g / l的Zn，约10至约20g / l的P 2 O 5，至少一种促进剂和约80至约220mg的磷酸盐溶液获得具有高覆盖系数的均匀磷酸盐层 /氟化物（“F（el）”），其通过浸入浴溶液中的氟化物敏感电极测定，其中游离酸（FA）的含量（以点计）已被调节并保持在值 对应于FA =（0.5〜1.0）+ K，其中K被计算为K =（0.002至0.012）×F（el）。 优选将游离酸（FA）含量调节至FA =（0.04〜0.06）×CP2O5 + K，并且使用K =（0.003〜0.009）×F（el）求出游离酸（FA）的含量。 该方法特别适于制备用于涂漆的表面，优选通过电泳浸涂。
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